CN114364472A - Additive manufacturing metal powder, additive manufacturing, and method of preparing additive manufacturing metal powder - Google Patents
Additive manufacturing metal powder, additive manufacturing, and method of preparing additive manufacturing metal powder Download PDFInfo
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- CN114364472A CN114364472A CN201980098571.4A CN201980098571A CN114364472A CN 114364472 A CN114364472 A CN 114364472A CN 201980098571 A CN201980098571 A CN 201980098571A CN 114364472 A CN114364472 A CN 114364472A
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Images
Classifications
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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
- B22F1/12—Metallic powder containing non-metallic particles
-
- 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
Abstract
A method of preparing an additive manufactured metal powder, comprising the steps of: decomposing the metal base powder into a metal alloy powder matrix (20) by a mechanical milling process; adding reinforcing particles (30) to a metal alloy powder matrix, and mixing the metal alloy powder matrix and the reinforcing particles to obtain composite metal particles (40), wherein the reinforcing particles are tantalum carbide or hafnium carbide, and the size range of the composite metal particles is 15-53 microns; adding a binder and binding the metal alloy powder matrix and the reinforcing particles together with the binder by a spray drying process to obtain dispersed particles; removing the binder from the dispersed particles by a sintering process to obtain an additive manufactured metal composite powder. The method enables the surface quality of components made of the additive manufactured composite metal powder and the fatigue properties thereof to be improved. Also relates to a powder produced by the above method and to a method of additive manufacturing.
Description
The invention relates to the field of additive manufacturing, in particular to additive manufacturing metal powder, additive manufacturing and a method for preparing the additive manufacturing metal powder.
Additive Manufacturing processes (Additive Manufacturing) are gaining increasing attention due to their rapid Manufacturing on a pre-designed based CAD model, which is capable of producing elements with complex shape structures in short look-ahead events. Selective Laser Melting (SLM) process is one of Additive manufacturing (Additive manufacturing) technologies that can be applied to metal and plastic materials. Where selective laser melting utilizes high power lasers to melt metal powders and build parts/components layer by layer through 3D CAD input, components with complex internal channels can be successfully fabricated.
Despite the promise of additive manufacturing techniques, challenges still exist to apply additive manufacturing techniques to critical components with desirable mechanical properties. Based on recent studies, in spite of having sufficient room temperature ductility properties, additively manufactured metallic materials generally show lower fatigue properties and higher high temperature creep properties. The reduction in grain size during high solidification rate additive manufacturing processes contributes to improved fatigue life, but also aggravates high temperature creep.
The additive manufacturing composite material can improve the function of the pure metal alloy if the reinforcing particles are added. For example, the reinforcing particles may further improve mechanical properties, wear and chemical resistance, thereby enabling critical components to be processed using additive manufacturing processes. Meanwhile, the reinforced particles of the traditional manufacturing process can improve the high-temperature creep property.
However, some typical reinforcing particles are carbide materials, such as tungsten carbide (WC) and titanium carbide (TiC). Due to the high-power laser adopted in additive manufacturing, the melting tank temperature can be higher than 2000 ℃, which is far higher than the decomposition temperature of the carbide, so that the carbide serving as a reinforcing particle can be decomposed. In addition, in order to reduce the brittle laves phase formed during the additive manufacturing process, the heat-resistant and high stress corrosion-resistant alloy usually needs to be solution heat treated at high temperature. For example, In718 materials are commonly used In additive manufacturing, and the heating process is performed at a temperature higher than 1100 ℃ and at a temperature higher than the normal decomposition temperature of the carbide material by 900 ℃. Also, since niobium (Nb) or nickel (Ni) has a stronger bonding force with carbon atoms, carbon atoms are generally more easily bonded with niobium (Nb) or nickel (Ni) during carbide decomposition of the heat and high stress resistant corrosion resistant alloy. The addition of tungsten carbide (WC) and titanium carbide (TiC) does not produce corresponding strengthening particles, but can deprive niobium (Nb) and nickel (Ni) elements in the alloy components. And Ni3Nb (gamma phase) composed of niobium (Nb) or nickel (Ni) is a main strengthening phase in the precipitation stage of the heat-resistant high-stress corrosion-resistant alloy. In addition, the formation of niobium carbide reduces the generation of a strengthening phase, thereby causing deterioration of high-temperature creep characteristics.
Although the carbide strengthening particles can act as pinning sites to hinder the generation and propagation of slip, thereby improving the mechanical strength of the material. However, if the reinforcing particles are oversized, they can cause defects like fatigue and cracks, promoting crack initiation and thus reducing the fatigue properties of the material. This is due to the different hardness of the large size reinforcing particles and the metal matrix, which if subjected to the same pulling force or deformation will slowly separate resulting in cracking. One of the solutions of the prior art is to select nano-reinforcing particles, but it is very difficult to obtain a uniform distribution of nano-reinforcing particles in the additively manufactured alloy. The uneven distribution of reinforcing particles in the additive manufactured metal composite also results in particle agglomeration and defect generation.
Disclosure of Invention
The invention provides a method for preparing additive manufacturing metal powder, which comprises the following steps: decomposing the metal base powder into a metal alloy powder matrix by a mechanical grinding process; adding reinforcing particles to a metal alloy powder matrix, and mixing the metal alloy powder matrix and the reinforcing particles to obtain composite metal particles, wherein the reinforcing particles are tantalum carbide or hafnium carbide, and the size range of the composite metal particles is 15-53 microns; adding a binder and binding the metal alloy powder matrix and the reinforcing particles together with the binder by a spray drying process to obtain dispersed particles; removing the binder from the dispersed particles by a sintering process to obtain an additive manufactured metal composite powder.
Further, the spray drying step comprises the following steps simultaneously or after the spray drying step: the dispersed particles are sieved to select the dispersed particles of a specific size.
Further, the mechanical grinding step further comprises the steps of: two or more metal base powders are respectively decomposed into metal alloy powder matrixes by a mechanical grinding process.
Further, the range of the particle size of the metal composite powder is 15 to 53 μm.
Furthermore, the range of the particle size of the enhanced particles is 50 nm-1 μm.
Further, the mixing step adopts a mechanical grinding process or an ultrasonic process.
Further, the reinforcing particles further include pure tantalum or pure hafnium.
Further, the additive manufacturing metal powder is prepared in selective laser melting equipment, wherein the laser power of the selective laser melting equipment ranges from 200W to 500W, and the scanning speed of the selective laser melting equipment ranges from 500mm/s to 2000 mm/s.
In a second aspect of the invention there is provided an additive manufactured metal powder, wherein the additive manufactured powder is produced by the method of the first aspect of the invention.
A third aspect of the invention provides an additive manufacturing method characterised in that it comprises a material produced by the method of the first aspect of the invention.
The particles of the metal powder provided by the invention have a circular shape and a controllable particle size, the particle size is close to 15-53 mu m, so the metal powder has good fluidity and is more suitable for a selective laser melting device. In the selective laser melting process, the composite metal powder is heated by laser energy and is immediately broken into distributed particles with the size of 50 nm-1 μm. The present invention can achieve a desired uniform particle strength to ensure a reinforcing effect and avoid defects due to non-uniform texture.
For fatigue fracture, crack initiation typically results in flaws or maximum effective size, such as pores or carbides. For the super heat-resistant high-stress corrosion-resistant alloy material manufactured by additive manufacturing, the maximum aperture value range is ten microns, which is much larger than that of nano reinforcing particles. The fatigue characteristic degradation effect by the reinforcing particles can be ignored. The components manufactured with the composite metal powder for additive manufacturing provided by the invention have good surface quality due to the use of nanoparticle fusion and improved fatigue properties.
In view of the relatively low stability and in view of the smaller bonding forces with carbon atoms in the carbide material, the present invention enables the selection of tantalum carbide (TaC) or hafnium carbide (HfC) which have a higher temperature stability and a higher degree of bonding with carbon atoms than niobium to reduce the possibility of niobium carbide formation. In addition, the invention adds tantalum or hafnium metal nano particles which can hold carbon atoms in niobium carbide to form carbonized reinforcing particles and release niobium atoms to obtain more Ni3Nb (gamma' phase).
FIG. 1 is a schematic view of a selective laser melting apparatus;
FIG. 2 is a schematic illustration of a method of making an additive manufactured metal powder according to a particular embodiment of the invention;
FIG. 3 is a schematic representation of the surface quality contrast of 3D prints made with and without metal powder added with reinforcing particles;
FIG. 4 is a schematic diagram of the creep strain comparison of 3D prints made with and without metal powder added with reinforcing particles;
fig. 5 is a schematic illustration of a method of making an additive manufactured metal powder according to yet another embodiment of the invention.
The following describes a specific embodiment of the present invention with reference to the drawings.
The present invention provides a composite powder for a selective laser melting apparatus, which can ensure uniform distribution of nano-reinforcing particles of an additive manufacturing alloy material.
Selective Laser Melting (SLM) is one of Additive manufacturing (Additive manufacturing) technologies that can rapidly manufacture the same parts as a CAD model by means of Laser sintering. Currently, selective laser melting processes are widely used. Unlike conventional material removal mechanisms, additive manufacturing is based on a completely opposite material additive manufacturing philosophy, in which selective laser melting utilizes high power lasers to melt metal powders and build up parts/components layer by layer through 3D CAD input, which can successfully manufacture components with complex internal channels.
FIG. 1 is a schematic view of a selective laser melting apparatus. As shown in FIG. 1, selective laser melting apparatus 100 includes a laser source 110, a mirror scanner 120, a prism 130, a powder feed cylinder 140, a forming cylinder 150, and a recovery cylinder 160. Therein, a laser source 110 is arranged above the selective laser melting apparatus 100, acting as a heating source for the metal powder, i.e. melting the metal powder for additive manufacturing.
Wherein, the powder feeding cylinder 140 has a first piston (not shown) at a lower portion thereof, which can move up and down, and the spare metal powder is placed in a cavity space above the first piston of the powder feeding cylinder 140, and the metal powder is fed from the powder feeding cylinder 140 to the molding cylinder 150 in accordance with the up and down movement of the first piston. In the forming cylinder 150, an additive manufacturing part placing table 154 is provided, one additive manufacturing part C is clamped above the placing table 154, and a second piston 152 is fixed below the placing table 154, wherein the second piston 152 and the placing table 154 are vertically arranged. During the additive manufacturing process, the second piston 152 moves from top to bottom to form a printing space in the forming cylinder 220. The laser source 110 for laser scanning should be disposed above the forming cylinder 150 of the selective laser melting apparatus, and the mirror scanner 120 adjusts the position of the laser by adjusting the angle of one prism 130, and determines which region of the metal powder is melted by the laser by adjusting the prism 130. The powder feeding cylinder 140 further includes a roller (not shown), and the metal powder P is stacked on an upper surface of the first piston, which vertically moves from bottom to top to transfer the metal powder to an upper portion of the powder feeding cylinder 140. The selective laser melting apparatus 100 further includes a roller, by which the additive manufacturing powder can be laid down for the forming cylinder 220. The roller may roll on the metal powder P to feed the metal powder P into the forming cylinder 150. And continuously performing laser scanning on the metal powder, decomposing the metal powder into a powder matrix, and continuously performing laser scanning on the powder matrix until the powder matrix is sintered into a printing piece C with a preset shape from bottom to top. In addition, the selective laser melting apparatus 100 further includes a recycling cylinder 160, and the recycling cylinder 160 is used to recycle the used metal powder in the forming cylinder 150.
The method for preparing the additive manufacturing metal powder comprises the following steps:
step S1 is first performed to decompose the metal base powder into metal alloy base powder by a mechanical grinding process (mechanical grinding). In particular, the metal powder is soaked in a solvent to prevent oxidation of the powder during the milling stage. Specifically, mechanical grinding includes especially ball grinding (ball mill), which is a process for grinding and mixing materials, widely used in painting paints (paintings), fireworks manufacturing (pyrotechnics), ceramics (ceramics), and selective laser sintering (selective laser sintering). The ball mill comprises a hollow cylindrical housing rotating about an axis, the axis of the hollow cylindrical housing being horizontal or substantially horizontal, and partially filling the ball. Specifically, the grinding medium of the ball grinding technology is a sphere, and the material of the sphere is steel (chrome steel), stainless steel or ceramic. The inner surface of the cylindrical shell is typically conformed with a wear resistant material, including manganese steel or ceramic. The force in grinding is provided by the balls in the cylindrical housing falling off the top of the housing, thereby reducing the size of the material being ground.
As shown in fig. 2, according to an embodiment of the present invention, step S1 is first performed to decompose the metal base powder into a metal alloy powder matrix through a mechanical milling process. Wherein, IN this embodiment, the metal base powder comprises a metal alloy powder that is a small size superalloy powder, such as IN 718. In this step, the metal base powder is decomposed into the metal alloy powder matrix 20. Wherein the size range of the metal alloy powder matrix is 50 nm-1 μm. The dispersed metal matrix particles and reinforcing particles of a predetermined size can be obtained by mechanically milling a liquid powder, such as liquid methanol. In addition, the brittleness of the particles can be improved through liquid nitrogen, so that the grinding efficiency is improved. The grinding time depends, among other things, on the type and efficiency of the metal matrix powder.
Then, step S2 is executed, reinforcing particles are added to the metal alloy powder matrix, and the metal alloy powder matrix and the reinforcing particles are mixed to obtain composite metal particles 40, wherein the reinforcing particles are tantalum carbide or hafnium carbide 30, and the size of the composite metal particles ranges from 15 micrometers to 53 micrometers. Specifically, the process adopted in the mixing step S2 is a mechanical grinding process or an ultrasonic process. The present invention can simultaneously accomplish the step of decomposing the metal alloy powder matrix into small-sized metal alloy powder matrices and the step of mixing the metal alloy powder matrices and the reinforcing particles in the mechanical grinding process without additionally providing a mixing step. According to a variant of the invention, after performing the mechanical grinding step S1, the metal powder matrix and the reinforcing particles are mixed using an ultrasonic process. Specifically, in the present embodiment, as shown in fig. 3, the powder mixed at this time includes the metal alloy powder matrix 20 and the reinforcing particles. At this time, the metal alloy powder matrix 20 and the reinforcing particles are also present in the liquid in the mixed powder. Specifically, the ground metal alloy powder matrix 20 and the reinforcing particles are mixed together in a short time mechanical grinding or ultrasonic process to obtain a uniform distribution of the reinforcing particles, and the amount of reinforcement is adjusted by a predetermined ratio of the reinforcing particles.
The reinforcing particles function to fix grain boundaries in the crystal, reduce deformation of the grains and generation and expansion of slip bands, thereby enhancing material strength and hindering generation of cracks in the final 3D print. Fig. 3 is a metallographic photograph of a sample with and without added reinforcing particles, wherein P1 is without added reinforcing particles and P2 is with added reinforcing particles. As shown in FIG. 3, P1 has larger crystal grains, while P2 has smaller crystal grains after adding the reinforcing particles, so that the crystal grains are refined, and the strength of the material is improved.
FIG. 4 is a graph showing the comparison of creep strain with and without the addition of reinforcing particles, where the abscissa is time and the ordinate is creep strain. As shown in fig. 4, a curve S1 is a material creep strain curve to which the reinforcing particles are not added, and a curve S2 is a sample creep strain curve to which the reinforcing particles are added. Comparing curves S1 and S2, curve S2 shows lower creep strain at the same time and under the same temperature and applied force, so the addition of reinforcing particles increases creep resistance.
Next, step S3 is performed to add a binder and bond the metal alloy powder matrix and the reinforcing particles together with the binder through a spray drying process, thereby obtaining dispersed particles. Specifically, as shown in fig. 2, the binder is used to bind the mixed powder including the metal alloy powder matrix 20 and the reinforcing particles together into a larger-sized powder. The spray drying process disperses the metal alloy powder matrix 20 and reinforcing particles that are bonded together by mechanical action into fine particles, "prilling," and then accelerates the drying process by increasing the area of water evaporation to remove most of the water, drying the bonded metal alloy powder matrix 20 and reinforcing particles into a powder. The metal alloy powder matrix 20 and the reinforcing particles, which are bonded together, are in a liquid, in the form of a slurry, prior to passing through the spray drying process, and a substantial portion of the water is removed after passing through the spray drying process, resulting in dried dispersed particles 50. Among them, since a binder is added to the slurry, the composite particles can be prepared by spray drying (spray drying) and have dispersed particles. The size of the composite particles will be controlled by the parameters of the spray drying, including the selected sieve size. Finally, the composite powder is heated and degummed under a mixture of argon and hydrogen to remove the binder.
According to a variant of the above preferred embodiment, as shown in fig. 5, the reinforcing particles further comprise pure tantalum or pure hafnium 60. That is, in step S2, reinforcing particles are added to the metal alloy powder matrix 20, and the metal alloy powder matrix 20 and the reinforcing particles are mixed to obtain composite metal particles, wherein the reinforcing particles are tantalum carbide or hafnium carbide 30, and the reinforcing particles further include pure tantalum or pure hafnium 60. Next, step S3 is performed to add a binder and bond the metal alloy powder matrix 20 and the reinforcing particles tantalum carbide or hafnium carbide 30 and pure tantalum or pure hafnium 60 together with the binder through a spray drying process to obtain dispersed particles 50'.
Finally, step S4 is performed, and the adhesive in the dispersed particles is removed by a degumming process, so as to obtain the additive manufacturing metal composite powder. Specifically, the degumming process (sintering) is a process of heating the dispersed particles 50 or 50' and then cooling to room temperature. As a result of the degelation, the bonding between the components in the dispersed particles 50 or 50' occurs, the strength of the sintered body is increased, and the binder is removed, obtaining a metal composite powder that can be used for 3D printing. Among them, the degumming process needs to be performed in an argon (argon) or hydrogen (hydrogen) gas atmosphere in order to prevent oxidation of the particles.
Further, the spray drying step comprises the following steps simultaneously or after the spray drying step: the dispersed particles are sieved to select the dispersed particles of a specific size.
Further, the mechanical grinding step further comprises the steps of: two or more metal base powders are respectively decomposed into metal alloy powder matrixes by a mechanical grinding process.
Further, the range of the particle diameter of the metal composite powder is 15 μm to 53mm (what.
Further, the range of the particle size of the reinforcing particles is 50nm to 1 μm (what.
Further, the mixing step adopts a mechanical grinding process or an ultrasonic process.
Further, the additive manufacturing metal powder is prepared in selective laser melting equipment, wherein the laser power of the selective laser melting equipment ranges from 200W to 500W, and the scanning speed of the selective laser melting equipment ranges from 500mm/s to 2000 mm/s.
A second aspect of the invention provides an additive manufactured metal powder produced by the method provided by the first aspect of the invention.
A third aspect of the invention provides an additive manufacturing method, wherein the additive manufacturing method comprises the step of preparing an additive manufactured metal powder by the method of the first aspect of the invention.
The particles of the metal powder provided by the invention have a circular shape and a controllable particle size, the particle size is close to 15-53 mu m, so the metal powder has good fluidity and is more suitable for a selective laser melting device. In the selective laser melting process, the composite metal powder is heated by laser energy and is immediately broken into distributed particles with the size of 50 nm-1 μm. The present invention can achieve a desired uniform particle strength to ensure a reinforcing effect and avoid defects due to non-uniform texture.
For fatigue fracture, crack initiation typically results in flaws or maximum effective size, such as pores or carbides. For the super heat-resistant high-stress corrosion-resistant alloy material manufactured by additive manufacturing, the maximum aperture value range is ten microns, which is much larger than that of nano reinforcing particles. The fatigue characteristic degradation effect by the reinforcing particles can be ignored. The components manufactured with the composite metal powder for additive manufacturing provided by the invention have good surface quality due to the use of nanoparticle fusion and improved fatigue properties.
In view of the relatively low stability and in view of the smaller bonding forces with carbon atoms in the carbide material, the present invention enables the selection of tantalum carbide (TaC) or hafnium carbide (HfC) which have a higher temperature stability and a higher degree of bonding with carbon atoms than niobium to reduce the possibility of niobium carbide formation. In addition, the invention adds tantalum or hafnium metal nano particles which can hold carbon atoms in niobium carbide to form carbonized reinforcing particles and release niobium atoms to obtain more Ni3Nb (gamma' phase).
While the present invention has been described in detail with reference to the preferred embodiments, it should be understood that the above description should not be taken as limiting the invention. Various modifications and alterations to this invention will become apparent to those skilled in the art upon reading the foregoing description. Accordingly, the scope of the invention should be determined from the following claims. Furthermore, any reference signs in the claims shall not be construed as limiting the claim concerned; the word "comprising" does not exclude the presence of other devices or steps than those listed in a claim or the specification; the terms "first," "second," and the like are used merely to denote names, and do not denote any particular order.
Claims (10)
- A method of preparing an additive manufacturing metal powder, comprising the steps of:decomposing the metal base powder into a metal alloy powder matrix by a mechanical grinding process;adding reinforcing particles to a metal alloy powder matrix, and mixing the metal alloy powder matrix and the reinforcing particles to obtain composite metal particles, wherein the reinforcing particles are tantalum carbide or hafnium carbide, and the size range of the composite metal particles is 15-53 microns;adding a binder and binding the metal alloy powder matrix and the reinforcing particles together with the binder by a spray drying process to obtain dispersed particles;removing the binder from the dispersed particles by a sintering process to obtain an additive manufactured metal composite powder.
- The method of making an additive manufactured metal powder of claim 1, further comprising, simultaneously with or after the spray drying step, the steps of: the dispersed particles are sieved to select the dispersed particles of a specific size.
- The method of making an additive manufactured metal powder of claim 1, wherein the step of mechanically milling further comprises the steps of: two or more metal base powders are respectively decomposed into metal alloy powder matrixes by a mechanical grinding process.
- The method of preparing an additive manufactured metal powder of claim 1, wherein the particle size of the metal composite powder ranges from 15 μ ι η to 53 μ ι η.
- The method of claim 1, wherein the reinforcing particle size ranges from 50nm to 1 μ ι η.
- The method of preparing an additive manufactured metal powder of claim 1, wherein the mixing step employs a process that is a mechanical milling process or an ultrasonic process.
- The method of making an additive manufactured metal powder of claim 1, wherein the reinforcing particles further comprise pure tantalum or pure hafnium.
- The method of preparing an additive-manufactured metal powder of claim 1, wherein the additive-manufactured metal powder is prepared in a selective laser melting apparatus, wherein a laser power of the selective laser melting apparatus ranges from 200W to 500W, and a scan rate of the selective laser melting apparatus ranges from 500mm/s to 2000 mm/s.
- Additive manufacturing metal powder, wherein the additive manufacturing powder is prepared by the method of any one of claims 1 to 8.
- Additive manufacturing method, characterized in that it comprises the step of preparing an additive manufactured metal powder by the method of any of claims 1 to 8.
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| PCT/CN2019/103636 WO2021035677A1 (en) | 2019-08-30 | 2019-08-30 | Additive manufacturing metal powder, additive manufacturing, and method for preparing additively manufactured metal powder |
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| CN114054761A (en) * | 2021-11-17 | 2022-02-18 | 株洲硬质合金集团有限公司 | Preparation method of metal ceramic powder for 3D printing |
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