Method, equipment and system for manufacturing modified lead apatite
By introducing copper nanoparticles into lead apatite materials and melting and superposition using additive manufacturing technology, combined with quenching treatment, the problems of lead apatite materials in forming control, structural refinement and electrical conductivity improvement are solved, and the manufacturing of high-performance lead apatite components is realized.
Patent Information
- Application Number
- CN202311089328.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-08-28
- Publication Date
- 2025-05-06
- Estimated Expiration
- 2043-08-28
AI Technical Summary
The existing lead apatite manufacturing methods are difficult to achieve personalized forming control, microstructure refinement and high-strength performance improvement, and have poor conductivity, which cannot meet the needs of high-performance applications.
Modified lead apatite parts are constructed layer by mixing copper nanoparticles with spherical lead apatite powder particles and melting and superposition using laser beams in additive manufacturing equipment, and quenching is performed to improve the conductive properties and structural density of the material.
It realizes personalized forming control, microstructure refinement and high-strength performance improvement of lead apatite materials, while significantly improving the conductive properties of the materials to meet the needs of high-performance applications.
Smart Images

Figure CN117020228B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to a method for manufacturing modified lead apatite, and more particularly to a method for manufacturing modified lead apatite by an additive manufacturing process. Background Art
[0002] Existing lead apatite is often formed into powder and then sintered to obtain a lead apatite product of a specific shape. In this forming process, it is difficult to ensure the personalized forming control of the lead apatite material. At the same time, due to the sintering forming, the product microstructure is coarse, which is difficult to meet the growing demand for high-strength personalized parts products.
[0003] With the continuous advancement of industry and technology, the demand for personalized, high-strength and high-performance parts is increasing. However, the traditional lead apatite manufacturing method has limitations that hinder its application in meeting these needs. The powder forming and sintering processes limit the shape and microstructure control of lead apatite materials, resulting in insufficient performance of the product in high-strength scenarios. Severe deformation during powder forming and grain growth during sintering may also lead to instability in the shape and size of the product. In addition, the electrical conductivity of traditional lead apatite materials is relatively poor, which limits its application in certain high-performance applications.
[0004] Therefore, seeking an innovative manufacturing method that can achieve personalized forming control, microstructure refinement and improvement of high-strength performance of lead apatite, so as to produce lead apatite components with more uniform distribution of nano-copper particles and change the conductive properties of lead apatite is crucial for the further development of lead apatite materials. Summary of the invention
[0005] In order to manufacture lead apatite components with more uniform distribution of nano-copper particles and change the conductive properties of lead apatite, the first aspect of the present application provides a method for manufacturing modified lead apatite, comprising: filling the provided copper nanoparticles and spherical lead apatite powder particles into an additive manufacturing device according to a preset combining process to form a flat raw material powder on a powder bed, controlling a laser beam to move along a predetermined scanning trajectory to melt the raw material powder at corresponding positions on the powder bed, and stacking them layer by layer into a modified lead apatite part; and quenching the formed modified lead apatite part to obtain the final form of the modified lead apatite.
[0006] Preferably, the preset combining process includes: before filling into the additive manufacturing equipment, using a planetary mixer to mix the copper nanoparticles and the spherical lead apatite powder particles, and / or using a ball mill to ball mill the copper nanoparticles and the spherical lead apatite powder particles to obtain raw material powder.
[0007] Preferably, during the powder mixing process of the copper nanoparticles and the spherical lead apatite powder particles, an inert gas is introduced into the powder mixing space.
[0008] Preferably, the preset combining process includes: filling spherical lead apatite powder particles into an additive manufacturing device and laying them on a powder bed; and infiltrating the prepared copper nanoparticle suspension on the powder bed to deposit it on the surface and / or inside of the spherical lead apatite powder to obtain a raw powder, wherein the copper nanoparticle suspension is prepared using at least copper nanoparticles.
[0009] Preferably, during the infiltration of the copper nanoparticle suspension, the copper nanoparticles and the spherical lead apatite powder particles are allowed to interact and gradually fuse with each other by means of laser beam irradiation and preheating.
[0010] Preferably, the trajectory of the laser beam irradiation preheating is the same as the predetermined scanning trajectory, and the area of the laser beam irradiation preheating is at least equal to the area covered by the predetermined scanning trajectory.
[0011] Preferably, the particle size of the spherical lead apatite powder particles is 5-90 μm, and the D50 particle size is 50 μm.
[0012] Preferably, the quenching process includes: placing the modified lead apatite parts in a heat treatment furnace, raising the furnace temperature to 750-800° C., keeping the temperature for 2 hours, and then performing quenching treatment, and the cycle is repeated 2-3 times.
[0013] Preferably, the atomic ratio of the copper nanoparticles to the lead element in the spherical lead apatite powder particles is 0.5-5:1.
[0014] Preferably, when the laser beam moves along a predetermined scanning trajectory, the laser scanning speed is 50-500 mm / s, the laser power is 200-500 W, and the depth of the molten pool formed by scanning is 100-150 μm.
[0015] The modified lead apatite constructed by the manufacturing method provided in the present application aims to promote the improvement of the electrical conductivity of the lead apatite material through the uniform distribution of copper nanoparticles and the lattice changes induced by heat treatment. The electrical conductivity of the modified lead apatite material can be enhanced by adjusting the lattice structure and element occupancy.
[0016] The second aspect of the present application provides an additive manufacturing device, comprising: at least one powder bin for storing raw material powder formed by combining copper nanoparticles and spherical lead apatite powder particles, wherein the raw material powder is combined by using a planetary mixer to mix the copper nanoparticles and the spherical lead apatite powder particles, and / or by using a ball mill to form the copper nanoparticles and the spherical lead apatite powder particles; a powder spreading device for spreading the raw material powder overflowing from the powder bin onto a powder bed; and an optical path unit for controlling a laser beam to move along a predetermined scanning trajectory to melt the raw material powder at a corresponding position on the powder bed, stacking layers into modified lead apatite parts, wherein the formed modified lead apatite parts are quenched to obtain the modified lead apatite in a final form.
[0017] The third aspect of the present application provides an additive manufacturing device, including: at least one powder bin for storing spherical lead apatite powder particles; a powder spreading device for spreading the spherical lead apatite powder particles overflowing from the powder bin onto a powder bed; an infiltration device for infiltrating a prepared copper nanoparticle suspension onto the powder bed so that it is deposited on the surface and / or inside of the spherical lead apatite powder to obtain a raw material powder, wherein the copper nanoparticle suspension is prepared using at least copper nanoparticles; and an optical path unit for controlling a laser beam to move along a predetermined scanning trajectory to melt the raw material powder at a corresponding position on the powder bed, stacking layers into modified lead apatite parts, wherein the formed modified lead apatite parts are quenched to obtain the modified lead apatite in a final form.
[0018] Preferably, the optical path unit is used to make the copper nanoparticles interact with the spherical lead apatite powder particles and gradually fuse them by preheating them through laser beam irradiation during the infiltration process of the copper nanoparticle suspension.
[0019] The fourth aspect of the present application provides a system, comprising: a planetary mixer; a ball mill; a quenching device; and the additive manufacturing equipment provided in the second aspect.
[0020] The fifth aspect of the present application provides a system, comprising: a quenching device; and the additive manufacturing device provided in the third aspect. BRIEF DESCRIPTION OF THE DRAWINGS
[0021] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on the provided drawings without paying creative work.
[0022] Figure 1 The figure shows the process of the method for manufacturing modified lead apatite provided by one or more embodiments of the present application;
[0023] Figure 2 What is shown is the state of the powder mixing space provided by one or more embodiments of the present application;
[0024] Figure 3 The structure of an additive manufacturing device provided by one or more embodiments of the present application is shown;
[0025] Figure 4 Shown is the molten pool morphology provided by one or more embodiments of the present application;
[0026] Figure 5 The figure shows the process of the method for manufacturing modified lead apatite provided by one or more embodiments of the present application;
[0027] Figure 6 The structure of an additive manufacturing device provided by one or more embodiments of the present application is shown;
[0028] Figure 7 The figure shows the powder dipping process of the dipping device provided by one or more embodiments of the present application;
[0029] Figure 8 , 9 Shown respectively are the structures of the modified lead apatite manufacturing system provided by one or more embodiments of the present application. DETAILED DESCRIPTION
[0030] Embodiments of the present invention are described in detail below, examples of which are shown in the accompanying drawings, wherein the same or similar reference numerals throughout represent the same or similar elements or elements having the same or similar functions. The embodiments described below with reference to the accompanying drawings are exemplary and are intended to be used to explain the present invention, and should not be construed as limiting the present invention.
[0031] The term "additive manufacturing equipment" as used in this context refers to 3D printing equipment, in particular powder-laying 3D printing equipment, and in particular equipment that forms parts using SLS (selective laser sintering) or SLM (selective laser melting) technology; wherein SLM is the preferred use scheme of the present invention, and the manufacturing process of this type of equipment involves scanning cross-sections of the material on a powder bed, using a laser beam to selectively fuse the powdered material, and scanning these cross-sections based on a three-dimensional description of the desired part; the source of the three-dimensional description is, for example, a computer-aided design (CAD) file, scanned data, or some other source.
[0032] "Lead apatite" used in this context refers to an ore whose chemical composition mainly includes lead, phosphorus and oxygen, among which lead element occupies the major part of the ore. Lead apatite is a kind of phosphate mineral in geology, and usually appears in yellow-green or brown crystalline form.
[0033] On the one hand, the present invention discloses a method for manufacturing modified lead apatite, which comprises filling provided copper nanoparticles and spherical lead apatite powder particles into an additive manufacturing device according to a preset combining process to form a flat raw material powder on a powder bed, controlling a laser beam to move along a predetermined scanning trajectory to melt the raw material powder at a corresponding position on the powder bed, and stacking them layer by layer to form a modified lead apatite part; and quenching the formed modified lead apatite part to obtain the final form of the modified lead apatite.
[0034] FIG. 1 shows an embodiment of a method 10 for manufacturing modified lead apatite, the implementation of which relies on steps S11 to S14.
[0035] S11. Combining the provided copper nanoparticles with spherical lead apatite powder particles to form a raw material powder.
[0036] Copper nanoparticles and spherical lead apatite powder particles are obtained as processing raw materials. The copper nanoparticles can be prepared by a chemical synthesis method to ensure that they have a uniform particle size distribution and required properties; the spherical lead apatite powder particles can be obtained by mechanical grinding; the obtained copper nanoparticles are mixed with the spherical lead apatite powder particles so that the two particles with different properties are evenly combined together. The mixing can be completed by mechanical stirring, shaking, crushing and the like.
[0037] In an exemplary embodiment, the particle size of the spherical lead apatite powder particles is 5-90 μm, and the D50 particle size is 50 μm. The D50 particle size represents the median of the particle size, and the D50 particle size of the spherical lead apatite powder particles is 50 μm, which means that in the particle size distribution, about half of the particles are smaller than 50 μm, and the other half are larger than 50 μm.
[0038] In an exemplary embodiment, the atomic ratio of the copper nanoparticles to the lead element in the spherical lead apatite powder particles is 0.5-5:1.
[0039] In some embodiments, a planetary mixer is used to mix copper nanoparticles and spherical lead apatite powder particles, and then a ball mill is used to mill the mixed copper nanoparticles and spherical lead apatite powder particles to obtain raw powder. Of course, the material mixed by the planetary mixer can also be directly used as the raw powder.
[0040] Figure 2The state of the powder mixing space 411 is shown. The planetary mixer has a powder mixing space 411. The particles in the powder mixing space 411 are mixed by rotation and collision. In this process, the copper nanoparticles 11 and the spherical lead apatite powder particles 12 are dispersed and mixed with each other to ensure uniform distribution during the entire mixing process. The mixed particles need to be further processed to obtain the required particle size and uniformity. In this process, a ball mill can be used to ball mill the mixed copper nanoparticles 11 and the spherical lead apatite powder particles 12. In the ball mill, the particles roll, collide and rub together with the ball mill (usually metal balls) in the container, gradually breaking and refining, and the mixing degree between the particles will also be further improved.
[0041] refer to Figure 2 In some embodiments, during the powder mixing process of the copper nanoparticles 11 and the spherical lead apatite powder particles 12, an inert gas is introduced into the powder mixing space 411, wherein the inert gas exemplarily includes nitrogen (N2), argon (Ar), helium (He) and a mixture thereof; in a preferred embodiment, the inert gas is argon. By introducing an inert gas into the powder mixing space 411, the presence of oxygen can be effectively reduced, and the risk of oxidation of the particles can be reduced. In addition, the inert gas helps to maintain the original properties of the particles and avoid chemical reactions that may occur in the presence of oxygen, which may affect their properties.
[0042] S12. Fill the combined raw material powder into the additive manufacturing equipment and lay it on the powder bed.
[0043] Figure 3 A configuration scheme of an additive manufacturing device 30 is shown. After the combined raw material powder 13 (a mixture of copper nanoparticles 11 and spherical lead apatite powder particles 12) is obtained, it is filled into the powder bin 31 of the additive manufacturing device 30. The powder bin 31 is a powder storage container for storing and supplying the raw material powder 13. The additive manufacturing device 30 is provided with a powder spreading device 32, which is used to evenly spread the raw material powder 13 overflowing from the powder bin 31 on the powder bed 35, that is, the powder spreading device 32 can control the flow and distribution of the powder to form a uniform layer of raw material powder 13 on the powder bed 35. Under the action of the upward drive of the powder bin 31, the raw material powder 13 rises from the powder bin 31 and overflows at the top. The overflowed raw material powder 13 will be guided by the powder spreading device 32 and evenly spread on the powder bed 35 to form a thin powder layer. The powder bed 35, as a part of the forming chamber 34, can be understood as a platform for building parts, which is supported by a movable platform in the forming chamber 34. The platform gradually descends during the construction of each layer so that a new powder layer can be laid and processed. The powder bed 35 is used to carry the raw material powder 13 and allow the laser or other processing methods to melt and superimpose the material on the powder layer.
[0044] In an exemplary embodiment, the powder coating thickness is 60-80 μm.
[0045] S13. Control the laser beam to move along a predetermined scanning trajectory to melt the raw material powder at the corresponding position on the powder bed, and stack them layer by layer to form a modified lead apatite part.
[0046] After the powder is laid, the laser beam is used to move along a predetermined scanning trajectory to melt the raw powder at a specific position on the powder bed. Through layer-by-layer laser scanning, the modified lead apatite parts of the desired shape are gradually constructed.
[0047] refer to Figure 3 The source of the laser beam is the optical path unit 33, which is mainly composed of a laser (generating a laser beam), a galvanometer (changing the propagation direction and angle of the laser beam) and a focusing lens (focusing the laser beam). The laser beam scanning parameters are set and the corresponding process control is realized through the logic control of the computer control system.
[0048] In an exemplary embodiment, when the laser beam moves along a predetermined scanning trajectory, the laser scanning speed is 50-500 mm / s, the laser power is 200-500 W, and the depth of the molten pool formed by scanning is 100-150 μm.
[0049] Figure 4 The morphology of the molten pool is shown. During the scanning process, a tiny molten pool will appear at the scanning position where the laser spot acts on the powder bed. The lead apatite powder particles will solidify very quickly after melting, and the copper nanoparticles will be quickly wrapped inside the lead apatite matrix, thereby obtaining a modified lead apatite structure.
[0050] In detail, when the laser beam is irradiated to a specific scanning position on the powder bed, due to the high energy density of the laser, the raw material powder reaches its melting point in a short time, forming a tiny molten pool. This molten pool is a local area where the powder particles are melted into a liquid state. Due to the high melting point of lead apatite, once the laser beam moves away, the melted lead apatite powder will quickly cool and solidify to form a solid structure. This fast solidification speed helps to maintain the shape of the powder in the molten pool area, thereby maintaining the accuracy and details of the built parts. Due to the relatively small size of copper nanoparticles, they may be quickly wrapped by the molten lead apatite matrix at the moment of laser irradiation. This is because the solidification speed of the lead apatite matrix is very fast, which will quickly wrap the molten copper nanoparticles and fix them inside the matrix. Due to the presence of copper nanoparticles, tiny particle dispersion areas may appear inside the melted lead apatite matrix. The copper nanoparticles in these areas may play a special role in the performance of the material, such as providing conductivity. This construction process is the key part of obtaining modified lead apatite materials.
[0051] S14. The formed modified lead apatite part is quenched to obtain the modified lead apatite in a final form.
[0052] The purpose of quenching is to optimize the crystal structure and performance of modified lead apatite parts by rapidly cooling the material from a high temperature state to a lower temperature. The formed modified lead apatite parts are first heated to a certain temperature, and then immersed in a cooling medium (such as oil, water or air, etc.) to cause the parts to be rapidly cooled. This rapid cooling rate leads to rapid solidification of the material, resulting in changes in the crystal structure to obtain the final form of the modified lead apatite parts.
[0053] In an exemplary embodiment, the quenching process is as follows: placing the modified lead apatite parts in a heat treatment furnace, raising the furnace temperature to 750-800° C., keeping the temperature for 2 hours, and then performing quenching treatment, and repeating the process 2-3 times.
[0054] The manufacturing method 10 proposed in this article mixes copper nanoparticles with spherical lead apatite powder particles, and ensures that the copper nanoparticles are fully mixed with the lead apatite powder particles by adopting processes such as planetary mixers and ball mills, thereby achieving uniform distribution of copper nanoparticles in the entire mixture.
[0055] In a subsequent stage of the manufacturing process, the copper nanoparticles are combined with the spherical lead apatite powder particles by laser melting, and based on a subsequent heat treatment, the part is heated to a certain temperature so that the copper atoms can partially replace the lattice sites of the lead atoms.
[0056] In detail, during heat treatment, copper atoms will find appropriate positions in the lead apatite lattice, replacing the positions of some lead atoms. This change in the lattice structure may affect the properties of the lead apatite material, especially the conductivity. The conductivity of lead apatite is related to its lattice structure and element occupancy. Through the partial substitution of copper atoms, the lattice structure changes, affecting the electronic band structure of the material, thereby affecting the conductivity; since copper has a high electrical conductivity, the presence of the replaced copper atoms in the lattice may promote the freer transmission of electrons within the material, thereby improving the conductivity of the material.
[0057] In summary, the modified lead apatite constructed by the manufacturing method provided in the present application aims to promote the improvement of the conductivity of the lead apatite material through the uniform distribution of copper nanoparticles and the lattice changes caused by heat treatment. The conductivity of the modified lead apatite material can be enhanced by adjusting the lattice structure and element occupancy.
[0058] FIG5 shows an implementation scheme of a method 20 for manufacturing modified lead apatite, the implementation of which relies on steps S21 to S24.
[0059] S21. Fill the provided spherical lead apatite powder particles into the additive manufacturing device and lay them on the powder bed.
[0060] Figure 6 The additive manufacturing device 30 is shown , A configuration scheme, after obtaining the spherical lead apatite powder particles 12, fill them into the additive manufacturing device 30 , Powder bin 31 , Inside, and through the powder spreading device 32 , From the powder bin 31 , The overflowed spherical lead apatite powder particles 12 are evenly laid on the powder bed 35 , Upper, namely powder spreading device 32 , By controlling the flow and distribution of powder, it can be achieved in the powder bed 35 , A uniform layer of spherical lead apatite powder particles 12 is formed on the surface.
[0061] S22. Infiltrating the prepared copper nanoparticle suspension on the powder bed to deposit it on the surface and / or inside of the spherical lead apatite powder to obtain a raw material powder, wherein the copper nanoparticle suspension is prepared using at least copper nanoparticles.
[0062] A copper nanoparticle suspension is prepared according to the provided copper nanoparticles 11. For example, the copper nanoparticles 11 can be dispersed in a suitable solvent to form a stable suspension. The copper nanoparticles 11 in the suspension should be evenly dispersed to ensure uniform particle deposition in the subsequent step.
[0063] Figure 7 FIG. 3 shows the powder dipping process of the infiltration device 36. In an exemplary embodiment, the prepared copper nanoparticle suspension 14 is stored and released by the infiltration device 36. Specifically, the copper nanoparticle suspension 14 stored inside is released by controlling the liquid outlet of the infiltration device 36 to fall onto the powder bed 35 below. , The copper nanoparticle suspension 14 penetrates into the pores and gaps of the spherical lead apatite powder particles 12 and is gradually deposited on the surface and / or inside of the spherical lead apatite powder particles 13 to combine therewith to form the raw material powder 13.
[0064] The infiltration device 36 should be able to , The spherical lead apatite powder particles 12 can be moved and lifted above the powder bed 35 when it is necessary to wet the spherical lead apatite powder particles 12 laid. , This requires the use of auxiliary tools, such as linear guide rails / electric lifting devices, etc. Exemplarily, the infiltration device 36 can be a device separated from the additive manufacturing device 30 , A separate device, of course, can also be designed as an additive manufacturing device30 ,part of the system to be controlled by a computer control system.
[0065] Exemplarily, the infiltration device 36 can be specifically a liquid injector, which is composed of a liquid delivery system and a nozzle, for example. The liquid delivery system can deliver the copper nanoparticle suspension from a storage container to the nozzle; when the suspension is sprayed through the nozzle, the liquid spray will be guided to the surface of the spherical lead apatite powder, and this process can be achieved by controlling the position, angle and injection pressure of the nozzle; when the liquid spray contacts the spherical lead apatite powder, the copper nanoparticles therein will be dispersed from the spray liquid to the surface and / or interior of the powder, and the tiny particles of the spray help to evenly introduce the copper nanoparticles into the powder.
[0066] In some optional embodiments, the copper nanoparticle suspension can be sprayed on the surface of the spherical lead apatite powder particles by inkjet. The infiltration device can be specifically a piezoelectric nozzle chamber, and the copper nanoparticle suspension in the chamber is ejected from the nozzle under the extrusion of the piezoelectric sheet, and the nozzle is controlled to be extruded in a specific area through an array of nozzles with the same width as the forming platform, so that the copper nanoparticle suspension can be sprayed on the forming platform / powder bed according to the preset area. In other words, by controlling the extrusion of the nozzle, the forming area on the forming platform / powder bed is pre-infiltrated, while other non-forming areas (non-laser scanning areas) are not infiltrated, thereby greatly saving the consumption of the copper nanoparticle suspension.
[0067] In some embodiments, during the infiltration process of the copper nanoparticle suspension, the copper nanoparticles and the spherical lead apatite powder particles are allowed to interact and gradually fuse by means of laser beam irradiation and preheating.
[0068] Preheating by laser irradiation to complete infiltration refers to the process of using laser irradiation to use the energy of the laser to make the copper nanoparticles interact with the lead apatite base material and gradually fuse, thereby introducing the copper nanoparticles into the lead apatite base material. By using a laser beam to irradiate the surface of the base material at a low power, although it is not enough to completely melt the base material, it can reach a sufficient temperature and some local melting, so that the copper nanoparticles can be locally infiltrated on the surface of the base material; during the laser preheating process, the copper nanoparticles are locally heated, may be partially melted, and then interact with the base material. Due to the thermal effect, the copper nanoparticles can gradually infiltrate and adhere to the surface / inside of the base material.
[0069] In an exemplary embodiment, the trajectory of the laser beam irradiation preheating is the same as the predetermined scanning trajectory, and the area of the laser beam irradiation preheating is at least equal to the area covered by the predetermined scanning trajectory.
[0070] During the additive manufacturing process, the predetermined build area and scanning trajectory are planned in advance. These scanning trajectories describe the path of the laser beam during the build process to achieve the melting and construction of the material on the powder bed. In order to achieve laser beam irradiation preheating, the equipment will move the laser beam along the same path as the predetermined scanning trajectory, which means that the laser beam will be preheated in the area that matches the actual build trajectory of the part; when the laser beam is preheated, the irradiation range of the laser beam is at least the same as the area covered by the predetermined scanning trajectory, or even larger, to ensure that the material in the entire build area is fully preheated, so that uniform melting and bonding can be achieved in the subsequent build process. By using the same trajectory as the build during the preheating process, it can also ensure that the temperature distribution in the build area is more uniform, and the uniformity of preheating helps to avoid possible thermal stress and deformation, and improve the overall quality of the built parts.
[0071] S23. Control the laser beam to move along a predetermined scanning trajectory to melt the raw material powder at the corresponding position on the powder bed, and stack them layer by layer to form a modified lead apatite part.
[0072] The laser beam is used to move along a predetermined scanning trajectory to melt the raw powder at a specific position on the powder bed. Through layer-by-layer laser scanning, the modified lead apatite parts of the desired shape are gradually constructed.
[0073] S24. The formed modified lead apatite parts are quenched to obtain the modified lead apatite in a final form.
[0074] It should be understood that the main difference between the modified lead apatite manufacturing method 20 provided by relying on S21-S24 and the modified lead apatite manufacturing method 10 provided by relying on S11-S14 is that the processes of combining copper nanoparticles and spherical lead apatite powder particles to obtain raw material powder are different. In method 10, copper nanoparticles and spherical lead apatite powder particles are mixed and / or ball-milled in advance to obtain raw material powder, and the raw material powder is filled into the powder bin of the additive manufacturing equipment for subsequent powder spreading and part assembly; while in method 20, only spherical lead apatite powder particles are filled into the powder bin, and then the spherical lead apatite powder particles are evenly spread on the powder bed by a powder spreading device. Only spherical lead apatite powder particles are involved in the material preparation stage, and the introduction of copper nanoparticles is achieved through the steps of suspension infiltration and / or laser irradiation preheating. In method 20, each time the powdering (spherical lead apatite powder particles) is performed, a suspension infiltration is required, that is, before each building layer, the copper nanoparticles are introduced into the powder bed using a suspension and deposited on the surface and / or inside of the spherical lead apatite powder particles to form a combined raw material powder.
[0075] The main effect of method 20 is that spherical lead apatite powder particles are filled into the powder bin and evenly spread on the powder bed by a powder spreading device, and then the copper nanoparticle suspension is introduced by laser irradiation preheating, so that it interacts with the lead apatite powder, and the copper nanoparticles are introduced layer by layer, which promotes the mutual fusion of the copper nanoparticles with the lead apatite matrix, thereby achieving the modification effect. This method can achieve uniform distribution and appropriate interaction of copper nanoparticles, and adjust the lattice structure and conductive properties in the modified lead apatite material finally constructed.
[0076] refer to Figure 3 On the one hand, this article discloses a manufacturing device for modified lead apatite, that is, an additive manufacturing device 30, which is composed of at least a powder bin 31, a powder spreading device 32, and an optical path unit 33, and also has a forming bin 34 provided with a powder bed 35 and a computer control system and other components.
[0077] The powder bin 31 is used to store the raw material powder 13 formed by combining copper nanoparticles and spherical lead apatite powder particles, wherein the combining process of the raw material powder 13 is to mix the copper nanoparticles and the spherical lead apatite powder particles using a planetary mixer, and / or to ball-mill the copper nanoparticles and the spherical lead apatite powder particles using a ball mill.
[0078] The powder spreading device 32 is used to spread the raw material powder 13 overflowing from the powder bin 31 onto the powder bed 35 .
[0079] The optical path unit 33 is used to control the movement of the laser beam along a predetermined scanning trajectory to melt the raw material powder 13 at the corresponding position on the powder bed 35, stacking layer by layer to form a modified lead apatite part. The formed modified lead apatite part is quenched to obtain the final form of modified lead apatite.
[0080] It should be understood that the additive manufacturing device 30 is used to perform at least a portion of the method 10 .
[0081] refer to Figure 6 On the one hand, this article discloses a manufacturing device for modified lead apatite, that is, an additive manufacturing device 30 , , which consists of at least one powder bin 31 , , powder spreading device 32 , , immersion device 36, optical path unit 33 , The composition also includes a powder bed 35 , Forming chamber 34 , And computer control system and other components.
[0082] The powder bin 31 is used to store the spherical lead apatite powder particles 12 .
[0083] Powder spreading device 32 , For removing powder from powder bin 31 ,The spherical lead apatite powder particles 13 overflowing from the powder bed 35 are laid on the powder bed 35. , superior.
[0084] The infiltration device 36 is used to infiltrate the prepared copper nanoparticle suspension 14 into the powder bed 35. , The copper nanoparticle suspension 14 is prepared by using at least copper nanoparticles, and is deposited on the surface and / or inside of the spherical lead apatite powder particles 12 to obtain raw material powder.
[0085] Optical path unit 33 , Used to control the laser beam to move along a predetermined scanning trajectory to melt the powder bed 35 , The raw material powders at corresponding positions above are stacked layer by layer to form modified lead apatite parts, wherein the formed modified lead apatite parts are quenched to obtain the final form of modified lead apatite.
[0086] Exemplarily, the optical path unit 33 , It is also used to make the copper nanoparticles interact with the spherical lead apatite powder particles 12 and gradually fuse them during the infiltration process of the copper nanoparticle suspension 14 by preheating with laser beam irradiation.
[0087] It should be understood that the additive manufacturing device 30 , It is used to perform at least a part of the implementation of method 20.
[0088] Figure 8 A configuration scheme of a modified lead apatite manufacturing system 40 is shown, which comprises a planetary mixer 41, a ball mill 42, a quenching device 43 and Figure 3 The additive manufacturing device 30 described is constructed.
[0089] It should be understood that the modified lead apatite manufacturing system 40 is used to perform all of the implementations of the method 10 .
[0090] Fig. 9 A modified lead apatite manufacturing system 40 is shown , A configuration scheme, the system 40 , By quenching equipment 43 and Figure 6 Additive manufacturing device described 30 , constitute.
[0091] It should be understood that the modified lead apatite manufacturing system 40 , It is used to execute all the implementations in method 20.
[0092] In the description of this specification, the description with reference to the terms "one embodiment", "some embodiments", "example", "specific example", or "exemplary embodiment" etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representations of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described may be combined in any one or more embodiments or examples in a suitable manner. In addition, those skilled in the art may combine and combine the different embodiments or examples described in this specification and the features of the different embodiments or examples, unless they are contradictory.
[0093] Although the embodiments of the present invention have been shown and described above, it is to be understood that the above embodiments are exemplary and are not to be construed as limitations of the present invention. A person skilled in the art may change, modify, replace and vary the above embodiments within the scope of the present invention.
[0094] Reference numerals list
[0095] 11 Copper Nanoparticles
[0096] 12 Spherical lead apatite powder particles
[0097] 13 Raw material powder
[0098] 14 Copper nanoparticle suspension
[0099] 30 ,30 , Additive Manufacturing Equipment
[0100] 31,31 , Powder silo
[0101] 32,32 , Powder spreading device
[0102] 33,33 , Optical path unit
[0103] 34,34 , Forming chamber
[0104] 35,35 , Powder Bed
[0105] 36 Infiltration device
[0106] 40,40 , Manufacturing Systems
[0107] 41 Planetary mixer
[0108] 411 Mixed Powder Space
[0109] 42 Ball Mill
[0110] 43,43 , Quenching equipment.
Claims
1. A method for producing modified lead apatite, characterized in that: The method comprises: The provided copper nanoparticles are combined with the spherical lead apatite powder particles according to a preset combining process to form a raw material powder, wherein the preset combining process includes: mixing the copper nanoparticles and the spherical lead apatite powder particles with a planetary mixer, and / or ball milling the copper nanoparticles and the spherical lead apatite powder particles with a ball mill to obtain the raw material powder; Filling the raw material powder into an additive manufacturing device to form a flat raw material powder on a powder bed, controlling the laser beam to move along a predetermined scanning trajectory to melt the raw material powder at a corresponding position on the powder bed, and stacking layers to form a modified lead apatite part; and The formed modified lead apatite parts are quenched to obtain the modified lead apatite in a final form.
2. The manufacturing method according to claim 1, characterized in that: During the powder mixing process of the copper nanoparticles and the spherical lead apatite powder particles, an inert gas is input into the powder mixing space.
3. A method for producing modified lead apatite, characterized in that: The method comprises: Filling the provided copper nanoparticles and spherical lead apatite powder particles into an additive manufacturing device according to a preset combining process to form a flat raw material powder on a powder bed, controlling a laser beam to move along a predetermined scanning trajectory to melt the raw material powder at a corresponding position on the powder bed, and stacking layers to form a modified lead apatite part; and The formed modified lead apatite parts are quenched to obtain the modified lead apatite in a final form.
4. The manufacturing method according to claim 3, characterized in that: The preset combining process includes: Filling the additive manufacturing device with spherical lead apatite powder particles and laying them on a powder bed; and The prepared copper nanoparticle suspension is infiltrated into a powder bed to deposit on the surface and / or inside of the spherical lead apatite powder to obtain the raw material powder, wherein the copper nanoparticle suspension is prepared using at least the copper nanoparticles.
5. The manufacturing method according to claim 4, characterized in that: During the infiltration process of the copper nanoparticle suspension, the copper nanoparticles and the spherical lead apatite powder particles are allowed to interact with each other and gradually fuse by means of laser beam irradiation and preheating.
6. The manufacturing method according to claim 5, characterized in that: The trajectory of the laser beam irradiation preheating is the same as the predetermined scanning trajectory, and the area of the laser beam irradiation preheating is at least equal to the area covered by the predetermined scanning trajectory.
7. The manufacturing method according to any one of claims 1 to 6, characterized in that: The particle size of the spherical lead apatite powder particles is 5-90 μm, and the D50 particle size is 50 μm.
8. The manufacturing method according to any one of claims 1 to 6, characterized in that: The quenching process includes: The modified lead apatite parts are placed in a heat treatment furnace, the furnace temperature is raised to 750-800° C., and quenching treatment is performed after keeping the temperature for 2 hours, and the cycle is repeated 2-3 times.
9. The manufacturing method according to any one of claims 1 to 6, characterized in that: The atomic ratio of the copper nanoparticles to the lead element in the spherical lead apatite powder particles is 0.5-5:
1.
10. The manufacturing method according to any one of claims 1 to 6, characterized in that: When the laser beam moves along a predetermined scanning trajectory, the laser scanning speed is 50-500 mm / s, the laser power is 200-500 W, and the depth of the molten pool formed by scanning is 100-150 μm.
11. An additive manufacturing device, characterized in that: include: At least one powder bin for storing raw material powder formed by combining copper nanoparticles and spherical lead apatite powder particles, wherein the raw material powder is combined by mixing the copper nanoparticles and the spherical lead apatite powder particles with a planetary mixer and / or by ball milling the copper nanoparticles and the spherical lead apatite powder particles with a ball mill; a powder spreading device, used for spreading raw material powder overflowing from the powder bin onto a powder bed; and An optical path unit is used to control the movement of a laser beam along a predetermined scanning trajectory to melt raw material powders at corresponding positions on a powder bed, and stack them layer by layer to form a modified lead apatite part, wherein the formed modified lead apatite part is quenched to obtain the final form of the modified lead apatite.
12. An additive manufacturing device, characterized in that: include: At least one powder bin for storing spherical lead apatite powder particles; a powder spreading device, used for spreading the spherical lead apatite powder particles overflowing from the powder bin onto the powder bed; an infiltration device, used for infiltrating the prepared copper nanoparticle suspension on the powder bed to deposit it on the surface and / or inside of the spherical lead apatite powder to obtain a raw material powder, wherein the copper nanoparticle suspension is prepared by at least using the copper nanoparticles; and An optical path unit is used to control the movement of a laser beam along a predetermined scanning trajectory to melt raw material powders at corresponding positions on a powder bed, and stack them layer by layer to form a modified lead apatite part, wherein the formed modified lead apatite part is quenched to obtain the final form of the modified lead apatite.
13. The additive manufacturing device according to claim 12, characterized in that: The optical path unit is also used to make the copper nanoparticles interact with the spherical lead apatite powder particles and gradually fuse them by means of laser beam irradiation preheating during the infiltration process of the copper nanoparticle suspension.
14. A modified lead apatite manufacturing system, characterized in that: include: A planetary mixer; A ball mill; - Quenching equipment; as well as The additive manufacturing apparatus of claim 11.
15. A modified lead apatite manufacturing system, characterized in that: include: - Quenching equipment; as well as The additive manufacturing apparatus according to claim 12 or 13.
Citation Information
Patent Citations
Preparation method for titanium alloy-hydroxyapatite salt biological ceramic porous material
CN108950305A
Porous titanium copper / hydroxyapatite composite material and preparation method
CN112853143A