Automatic high-flux micro-nano copper powder parallel synthesis and separation equipment

Abstract

The invention provides automatic high-flux micro-nano copper powder parallel synthesis and separation equipment, and relates to the technical field of metal powder preparation processes, the automatic high-flux micro-nano copper powder parallel synthesis and separation equipment comprises a support, a transfer device, a liquid preparation device, a reaction device and a separation device; the liquid preparation device is configured to bear a plurality of reagent bottles and sequentially supply reaction liquids with different proportions to the reagent bottles, the reaction device is provided with a plurality of reaction cavities for providing reaction environments for the reagent bottles respectively, and the separation device is provided with a plurality of separation holes for performing solid-liquid separation on reaction substances in the reagent bottles respectively; the transfer device is connected with the support and located above the first platform, and the transfer device is configured to transfer the reagent bottles in the X direction, the Y direction and the Z direction and transfer reacted substances in the reagent bottles to the separation device. The equipment has the advantages that high-flux automatic parallel synthesis and separation of the micro-nano copper powder can be realized, diversified research requirements of modern laboratories are met, the automation degree is high, the expansibility is good, human intervention is reduced, and the like.

Description

Technical Field

[0001] This invention relates to the field of metal powder preparation technology, and in particular to an automated high-throughput parallel synthesis and separation device for micro- and nano-copper powders. Background Technology

[0002] Micro- and nano-copper powders, due to their excellent electrical and thermal conductivity, catalytic activity, and good formability, have shown broad application prospects in fields such as electronics, chemical catalysis, powder metallurgy, and biomedicine. As related industries develop towards higher precision and integration, the demands on the morphology of micro- and nano-copper powders are constantly increasing, while more stringent requirements are being placed on their quality indicators such as particle size distribution uniformity, purity, and dispersibility. Micro- and nano-copper powders are increasingly widely used in multilayer ceramic capacitors, electronic pastes, and lubricant modifiers, playing a crucial role in improving the performance of electronic components.

[0003] Existing devices for preparing micro / nano copper powder have the following shortcomings: limited functionality, complex operation, and difficulty in high integration. For example, patent application number 202211466071.1 protects a method and device for preparing micro / nano copper powder, but the device only includes two liquid storage tanks and a microreactor, which cannot meet the diverse research needs of modern laboratories. In addition, since the solution preparation process requires manual operation, there are also problems such as many manual operations, high risk of sample contamination, low throughput, difficulty in processing multiple or several samples at the same time, and poor scalability. Summary of the Invention

[0004] This invention addresses the problems of low throughput, low parameter exploration efficiency, and easy cross-contamination between samples in existing micro / nano copper powder preparation devices. It provides an automated high-throughput parallel synthesis and separation device for micro / nano copper powder, which has the advantages of realizing high-throughput automated synthesis and separation of micro / nano copper powder, meeting the diverse research needs of modern laboratories, high degree of automation, good scalability, and reduced human intervention.

[0005] To achieve the above objectives, the present invention provides the following technical solution: This invention provides an automated high-throughput parallel synthesis and separation device for micro / nano copper powder, comprising a support, a transport device, a liquid preparation device, a reaction device, and a separation device; The support has a first platform, and at least a portion of the liquid preparation device, the reaction device, and the separation device are all mounted on the first platform. The solution preparation device is configured to hold multiple reagent bottles and sequentially supply reaction solutions with different ratios to each of the reagent bottles. The reaction apparatus is provided with multiple reaction chambers, each of which is used to provide an independent reaction environment for the corresponding reagent bottle; The separation device is provided with multiple separation holes, and each separation hole corresponds to the reaction chamber in terms of quantity and spatial position, for independent solid-liquid separation of the reacted substances in each reagent bottle. The transfer device is connected to the support and located above the first platform. The transfer device is configured to transfer the reagent bottle along the X, Y, and Z directions and sequentially complete the transfer operation between the solution preparation device, the reaction device, and the separation device according to a preset running path.

[0006] In an optional embodiment, the transfer device includes a first drive mechanism, a second drive mechanism, a third drive mechanism, and a first clamping mechanism; The first drive mechanism is mounted on the bracket and connected to the second drive mechanism, and the first drive mechanism is configured to drive the second drive mechanism to move along the Y direction; The second drive mechanism is connected to the third drive mechanism, and the second drive mechanism is configured to drive the third drive mechanism to move along the X direction; The third driving mechanism is connected to the first clamping mechanism. The third driving mechanism is configured to drive the first clamping mechanism to move along the Z direction. The first clamping mechanism is configured to pick up, place, and rotate the reagent bottle.

[0007] In an optional embodiment, the transfer device further includes a liquid suction mechanism; The liquid aspiration mechanism is detachably connected to a pipette tip for aspirating the reacted substances in the reagent bottles. The liquid aspiration mechanism transfers the reacted substances in each of the reagent bottles through the pipette tip. When transferring between different reagent bottles, the pipette tip can be replaced to achieve physical isolation between different reaction systems.

[0008] In an optional embodiment, the transfer device further includes a fourth drive mechanism; The fourth drive mechanism is connected to the second drive mechanism, and the second drive mechanism is further configured to drive the fourth drive mechanism to move independently of the third drive mechanism along the X direction. The fourth driving mechanism is connected to the liquid suction mechanism, and the fourth driving mechanism is configured to drive the liquid suction mechanism to move along the Z direction. The liquid suction mechanism is configured to transfer the reacted substance in the reagent bottle to the separation device.

[0009] In an optional embodiment, the automated high-throughput parallel synthesis and separation equipment for micro- and nano-copper powders further includes a pipette tip storage box and a pipette tip replacement assembly, both installed on the first platform. The pipette tip storage box stores a plurality of vertically placed pipette tips to be retrieved. The pipette tip replacement assembly has a rejection port for removing pipette tips from the liquid aspiration mechanism and a waste box located below the rejection port.

[0010] In an optional embodiment, a second clamping mechanism and a capping structure are also mounted on the first platform. The capping structure has a limiting cavity for accommodating the reagent bottle, and the second clamping mechanism is used to clamp the body of the reagent bottle.

[0011] In an optional embodiment, the liquid preparation device includes a liquid supply mechanism, a rotating mechanism, and a sample inlet plate; The rotating mechanism is installed on the first platform, the sample inlet disk is connected to the rotating mechanism, the sample inlet disk is provided with multiple supporting cavities along the circumference for supporting each of the reagent bottles, and the rotating mechanism is configured to drive the sample inlet disk to rotate.

[0012] In an optional embodiment, the liquid supply mechanism is connected to the support and has a liquid outlet located above the sample inlet plate, the liquid outlet being configured to sequentially supply reaction solutions of different proportions to each of the reagent bottles.

[0013] In an optional embodiment, the liquid supply mechanism includes a liquid storage assembly, a pump assembly, and a liquid addition assembly; The support has a second platform located below the first platform, and the liquid storage assembly is installed on the second platform. The liquid storage assembly is used to store multiple mother liquors. Both the pump assembly and the liquid addition assembly are mounted on the bracket. The pump assembly is connected between the liquid storage assembly and the liquid addition assembly. The pump assembly is configured to pump each of the mother liquors in the liquid storage assembly into the liquid addition assembly.

[0014] In an optional embodiment, the reaction apparatus includes a heating and stirring assembly and a protective cover; The heating and stirring assembly includes multiple reaction chambers, a magnetic field generator, and a heating platform located below the reaction chambers; The protective cover is configured to cover the heating and stirring assembly, and the protective cover has an air inlet configured to communicate with a protective gas source and an air outlet configured to communicate with an exhaust gas treatment device.

[0015] In an optional embodiment, the separation device includes a plate and a waste liquid tank; The plate is provided with a plurality of separation holes, and a filter membrane is provided in each separation hole; The waste liquid tank is sealed to the bottom of the plate and communicates with each of the separation holes. The waste liquid tank has an air extraction port configured to communicate with the pump body.

[0016] In optional embodiments, a cooling device and / or a sample holder may also be included; The cooling device is installed on the first platform, and the cooling device is provided with multiple cooling chambers for placing each of the reagent bottles; The sample rack is installed on the first platform, and the sample rack is provided with multiple sample slots for placing the various reagent bottles after the reaction.

[0017] In an optional embodiment, a control unit is also included, wherein the transfer device, the liquid preparation device, the reaction device, and the separation device are all connected to the control unit.

[0018] The automated high-throughput parallel synthesis and separation equipment for micro / nano copper powder provided by this invention does not simply increase the number of reactions. Instead, it addresses the problems of numerous reaction parameters, significant differences in manual operation, and easy cross-contamination between samples during the synthesis of micro / nano copper powder. It constructs an automated high-throughput system with a one-to-one correspondence between reaction and separation, operating independently in parallel. This ensures good comparability of micro / nano copper powder samples obtained under different reaction parameter conditions, thereby significantly improving process screening efficiency and experimental data reliability. The beneficial effects are not limited to the following: 1. Achieve high-throughput parallel automated synthesis and separation: By integrating the liquid preparation device, reaction device and separation device, and with the help of the transfer device that can move precisely in the X, Y and Z directions, the continuous liquid preparation, synchronous reaction and independent solid-liquid separation of reactants in multiple reagent bottles are realized, which significantly improves the experimental throughput, has good scalability and meets the needs of modern scientific research for diversified and batch sample processing.

[0019] 2. Supports parallel testing of multi-component and multi-ratio reaction conditions: The liquid preparation device can supply reaction solutions with different ratios to different reagent bottles. Combined with the reaction device with multiple reaction chambers, it enables the parallel execution of micro-nano copper powder synthesis experiments under multiple process parameters within the same operating cycle, enhancing the flexibility and research adaptability of the equipment.

[0020] 3. High degree of automation and reduced human intervention: The transfer device automatically completes the transfer of reagent bottles between various functional modules, including the transfer of post-reaction materials to the separation device, which effectively reduces the intensity of manual operation, avoids human error, and improves the accuracy and repeatability of experimental data. Attached Figure Description

[0021] To more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0022] Figure 1 This is a three-dimensional structural schematic diagram of the automated high-throughput parallel synthesis and separation equipment for micro / nano copper powder provided in an embodiment of the present invention; Figure 2 for Figure 1 A magnified view of part A; Figure 3 A side view of the automated high-throughput parallel synthesis and separation equipment for micro / nano copper powder provided in an embodiment of the present invention; Figure 4 A three-dimensional structural schematic diagram of the heating and stirring assembly provided in an embodiment of the present invention; Figure 5 This is a three-dimensional structural schematic diagram of the separation device provided in an embodiment of the present invention; Figure 6 A three-dimensional structural schematic diagram of the first clamping mechanism provided in an embodiment of the present invention; Figure 7 This is a three-dimensional structural diagram of the screw cap structure provided in an embodiment of the present invention; Figure 8 A three-dimensional structural schematic diagram of the liquid suction mechanism provided in an embodiment of the present invention; Figure 9 for Figure 1 A magnified view of part B; Figure 10 This is a three-dimensional structural schematic diagram of the cooling device provided in an embodiment of the present invention; Figure 11 This is a schematic diagram of the three-dimensional structure of the sample holder provided in an embodiment of the present invention; Figure 12 These are SEM images of the micro / nano copper powders synthesized in 24 experimental groups according to examples of this invention.

[0023] Icons: 1-Support; 11-First Platform; 12-Second Platform; 2-Transfer Device; 21-First Drive Mechanism; 22-Second Drive Mechanism; 23-Third Drive Mechanism; 24-First Clamping Mechanism; 241-Gripper; 242-Clamping Driver; 243-Rotary Drive Assembly; 25-Fourth Drive Mechanism; 26-Liquid Suction Mechanism; 261-Suction Head; 262-Liquid Storage Tube; 3-Liquid Dispensing Device; 31-Liquid Supply Mechanism; 311-Liquid Storage Assembly; 312-Pump Assembly; 313-Liquid Addition Assembly; 3131-Liquid Outlet; 32-Rotary Machine Structure; 33-Sample tray; 331-Bearing cavity; 4-Reaction device; 41-Heating and stirring assembly; 411-Reaction cavity; 412-Heating stage; 5-Separation device; 51-Plate body; 511-Separation hole; 52-Waste liquid tank; 6-Reagent bottle; 7-Biscuit tip storage box; 71-Biscuit tip to be picked up; 8-Biscuit tip replacement assembly; 81-Frame body; 811-Discarding port; 82-Waste box; 9-Second clamping mechanism; 10-Capping structure; 101-Limiting cavity; 011-Cooling device; 0111-Cooling cavity; 012-Sample rack; 0121-Sample slot. Detailed Implementation

[0024] The technical solution of the present invention will now be clearly and completely described with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0025] In the description of this invention, it should be noted that the terms "center," "upper," "lower," "left," "right," "vertical," "horizontal," "inner," and "outer," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are used only for the convenience of describing the invention and for simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on the invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and should not be construed as indicating or implying relative importance.

[0026] In the description of this invention, it should be noted that, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this invention according to the specific circumstances.

[0027] The specific embodiments of the present invention will be described in detail below with reference to the accompanying drawings. It should be understood that the specific embodiments described herein are for illustration and explanation only and are not intended to limit the present invention.

[0028] This embodiment provides an automated, high-throughput parallel synthesis and separation device for micro / nano copper powders, such as... Figures 1 to 5 As shown, it includes a support 1, a transfer device 2, a liquid preparation device 3, a reaction device 4, and a separation device 5. Under the coordinated control of the control unit, the liquid preparation device 3, the reaction device 4, and the separation device 5 execute according to the preset process parameter table, so as to complete the synthesis and separation of micro-nano copper powder under multiple different reaction ratios, reaction temperatures, and reaction times in the same operating cycle.

[0029] The support 1 has a first platform 11. At least part of the structure of the liquid preparation device 3, the reaction device 4, and the separation device 5 are mounted on the first platform 11. The liquid preparation device 3 is configured to carry multiple reagent bottles 6 and sequentially supply reaction solutions of different proportions to each reagent bottle 6 according to preset formula parameters. The reaction device 4 is provided with multiple reaction chambers 411 for providing a reaction environment for each reagent bottle 6. The separation device 5 is provided with multiple separation holes 511 for separating the reactants in each reagent bottle 6 into solid and liquid phases. Each separation hole 511 and the reaction chamber 411 form a one-to-one correspondence in number and spatial position, used for independent solid-liquid separation of the reacted substances in each reagent bottle 6. This device, by constructing a one-to-one correspondence between the reaction chambers 411 and the separation holes 511 in its structure and combining it with a transport device that can move independently in three-dimensional space, realizes the independent reaction and independent separation of multiple reaction systems within the same operating cycle, thereby avoiding mutual interference between samples. The transfer device 2 is connected to the support 1 and located above the first platform 11. The transfer device 2 is configured to transfer the reagent bottle 6 in the X, Y and Z directions, and according to the preset running path, it sequentially completes the transfer operation of the reagent bottle 6 between the liquid preparation device 3, the reaction device 4 and the separation device 5, so that each reagent bottle 6 runs along its own independent processing path during the liquid preparation, reaction and separation process, and finally realizes the transfer of the reacted substances in the reagent bottle 6 to the separation device 5.

[0030] In the automated high-throughput parallel synthesis and separation equipment for micro- and nano-copper powder provided in the above embodiments, the liquid preparation device 3 carries multiple reagent bottles 6 and sequentially provides reaction solutions with different ratios to each reagent bottle 6. At the same time, the transfer device 2 sequentially transfers each reagent bottle 6 containing the reaction solution to the reaction chamber 411 in the reaction device 4. After the transfer is completed, each reagent bottle 6 reacts in its respective reaction chamber 411. After the reaction is completed, the transfer device 2 transfers the reacted substances in the reagent bottles 6 to the separation device 5 for solid-liquid separation to obtain multiple portions of synthesized micro- and nano-copper powder.

[0031] The above-mentioned equipment integrates a liquid preparation device, a reaction device, and a separation device, and is equipped with a transfer device that can move precisely in the X, Y, and Z directions. It realizes continuous liquid preparation, synchronous reaction, and independent solid-liquid separation of reactants in multiple reagent bottles 6, which significantly improves experimental throughput, has good scalability, and meets the needs of modern scientific research for diversified and batch sample processing.

[0032] Among them, the liquid preparation device 3 can supply reaction solutions with different ratios to different reagent bottles 6. Combined with the reaction device 4 which has multiple reaction chambers 411, it enables the parallel execution of micro-nano copper powder synthesis experiments under multiple process parameters within the same operating cycle, thereby enhancing the flexibility and research adaptability of the equipment.

[0033] In addition, the transfer device 2 can automatically transfer the reagent bottle 6 between various functional modules, including the transfer of post-reaction materials to the separation device 5, which effectively reduces the intensity of manual operation, avoids human error, and improves the accuracy and repeatability of experimental data.

[0034] The structure of the transfer device 2 is described in detail below: In one alternative implementation, such as Figure 1 As shown, the transfer device 2 includes a first drive mechanism 21, a second drive mechanism 22, a third drive mechanism 23, and a first clamping mechanism 24. The first drive mechanism 21 is mounted on the bracket 1 and connected to the second drive mechanism 22, configured to drive the second drive mechanism 22 to reciprocate along the Y direction, forming a Y-axis motion system; the second drive mechanism 22 is connected to the third drive mechanism 23, configured to drive the third drive mechanism 23 to move along the X direction, forming an X-axis motion system; the third drive mechanism 23 is connected to the first clamping mechanism 24, configured to drive the first clamping mechanism 24 to move up and down along the Z direction, forming a Z-axis motion system. Thus, through the coordinated control of three orthogonal directions, the first clamping mechanism 24 can be precisely positioned to any specified location in three-dimensional space to complete the gripping, transporting, and placing operations of the reagent bottle 6.

[0035] Specifically, the first drive mechanism 21 may include a Y-axis guide rail and a Y-axis drive motor. The Y-axis drive motor drives the second drive mechanism 22 to slide along the Y-axis guide rail through a synchronous belt or lead screw transmission, ensuring smooth movement and high positioning accuracy.

[0036] The aforementioned first drive mechanism 21 can be configured as two, with the two first drive mechanisms 21 operating synchronously to support and drive the two ends of the second drive mechanism 22 to move along the Y direction.

[0037] Specifically, the second drive mechanism 22 can be integrated onto the moving end of the first drive mechanism 21. It has its own X-axis guide rail structure and a first X-axis drive motor. The first X-axis drive motor drives the third drive mechanism 23 to slide along the X-axis guide rail through a synchronous belt, lead screw transmission, or gear and rack transmission. Thus, through the coordinated work of the first drive mechanism 21 and the second drive mechanism 22, the two-dimensional spatial positioning function of the transfer device in the horizontal plane (XY plane) is realized.

[0038] The aforementioned first X-axis drive motor and Y-axis drive motor can be 86 stepper motors, with a positioning accuracy of ±0.2 mm.

[0039] Specifically, the third drive mechanism 23 may include a Z-axis linear module, a pneumatic / electric push rod, or a Z-axis drive motor. The Z-axis drive motor drives the first clamping mechanism 24 to slide along the Z-axis guide rail via a synchronous belt or lead screw transmission. The third drive mechanism 23 is installed at the output end of the second drive mechanism 22 and can respond to the command of the control unit to drive the first clamping mechanism 24 to rise or fall to a preset height position to adapt to the operational needs of different workstations.

[0040] The Z-axis drive motor mentioned above can be a 57-stepper motor, which is suitable for fine movements under small loads.

[0041] In addition, the first clamping mechanism 24 has clamping and releasing functions and is equipped with a rotary drive component, which enables it to drive the reagent bottle 6 to rotate around its own axis while in the clamping state. For example, the first clamping mechanism 24 can clamp the cap of the reagent bottle 6 and clamp the body of the reagent bottle 6 through other mechanisms to realize the tightening or loosening operation of the cap of the reagent bottle 6, further reducing the number of manual operations and facilitating the realization of fully automated operation.

[0042] Specifically, such as Figure 6 As shown, the first clamping mechanism 24 can achieve stepless rotation from 0 to 180° and an opening and closing stroke from 0 to 100 mm. Specifically, it can include a gripper 241, a clamping driver 242 (such as a miniature cylinder or servo motor), and a rotary drive assembly 243. The gripping driver 242 controls the opening and closing of the gripper 241 to achieve safe gripping and release of the reagent bottle 6; while the rotary drive assembly 243 is connected to the gripping driver 242 and is configured to drive the clamped reagent bottle 6 to rotate around its central axis.

[0043] The grippers can be made of 3D-printed titanium alloy (with a sandblasted surface and a slip resistance coefficient ≥0.8). A pressure sensor (range 0~50 N) can be installed inside the grippers to prevent excessive gripping force. The rotary drive assembly 243 can include a motor that drives the gripper 242, or it can be a combination of a motor and a transmission assembly, such as a belt drive assembly or a chain drive assembly.

[0044] The transfer device 2 provided in the above embodiment constructs a three-dimensional motion platform that can be independently controlled in the X, Y, and Z directions through the cascaded linkage of the first drive mechanism 21, the second drive mechanism 22, and the third drive mechanism 23. The motion stroke can be, but is not limited to, 1500 mm × 1200 mm × 500 mm, covering the working area formed by the first platform 11. In addition, the above-mentioned drive mechanisms, combined with the first clamping mechanism 24 which has pick-up, place-down, and rotation functions, realize the precise and automatic transfer of reagent bottles 6 between various functional modules, improving the automation level and operational reliability of the entire system.

[0045] In alternative implementations, such as Figure 1 and Figure 3 As shown, the automated high-throughput parallel synthesis and separation equipment for micro- and nano-copper powders also includes a second clamping mechanism 9 and a capping structure 10, both mounted on the first platform 11. The two work together to enable the automatic opening and closing of the caps on the reagent bottles 6 before and after the reaction, thereby further improving the automation level and operational safety of the equipment.

[0046] Specifically, such as Figure 7 As shown, the screw cap structure 10 is provided with a limiting cavity 101 for accommodating the reagent bottle 6. This limiting cavity 101 has a geometry adapted to the shape of the reagent bottle 6 (e.g., a cylindrical inner cavity), enabling axial positioning and radial limiting of the bottle body portion of the reagent bottle 6. The dimensions of the limiting cavity 101 must be designed to ensure that the upper area of ​​the bottle body and the cap are exposed within the limiting cavity 101 after the reagent bottle 6 is inserted.

[0047] Furthermore, such as Figure 3 As shown, the second clamping mechanism 9 is disposed on one side of the capping structure 10 and configured to radially clamp the body of the reagent bottle 6. The second clamping mechanism 9 includes at least one pair of openable and closable jaws. The inner side of the jaws may be provided with anti-slip texture or elastic padding to increase friction and avoid damage to the surface of the reagent bottle. The opening and closing action of the jaws is controlled by a pneumatic, electric or electromagnetic drive device.

[0048] In use, the first clamping mechanism 24 clamps the reagent bottle 6 after the reaction liquid has been injected and places the reagent bottle 6 into the limiting cavity 101 of the capping structure 10. Then, the second clamping mechanism 9 extends to clamp the body of the reagent bottle 6, and the first clamping mechanism 24 picks up the cap and aligns it with the bottle. The first clamping mechanism 24 then rotates the cap to connect the cap to the bottle body. Subsequently, the second clamping mechanism 9 releases its grip on the bottle body, and the first clamping mechanism 24, driven by the first driving mechanism 21, the second driving mechanism 22, and the third driving mechanism 23, places the reagent bottle 6 into the reaction cavity 411 of the reaction device 4. After the reaction of the reagent bottle 6 is completed, the first clamping mechanism 24 clamps the cap of the reagent bottle 6 and places the reagent bottle 6 into the limiting cavity 101. Then, the second clamping mechanism 9 extends to clamp the body of the reagent bottle 6, and the first clamping mechanism 24 rotates the cap in the opposite direction to disconnect the cap from the bottle body.

[0049] The above-described embodiment achieves stable clamping of the bottle body through the second clamping mechanism 9, effectively preventing the bottle body from rotating with the cap during the capping process, thus ensuring the reliability and consistency of the opening / closing operation. At the same time, the capping structure 10 and the second clamping mechanism 9 are both fixedly installed on the first platform 11, with a stable positional relationship, which facilitates spatial coordinate matching and action interlocking control with the transfer device 2, and is suitable for multi-batch, continuous micro-nano copper powder synthesis and separation scenarios.

[0050] In an optional embodiment, the transfer device 2 further includes a liquid suction mechanism 26, which is detachably connected to a pipette tip 261 for aspirating the reacted substance in the reagent bottle 6. The liquid suction mechanism 26 transfers the reacted substance in each reagent bottle 6 through the pipette tip 261. When transferring between different reagent bottles 6, the pipette tip 261 can be replaced to achieve physical isolation between different reaction systems.

[0051] Specifically, the suction head 261 has a liquid suction channel and a terminal opening, which can complete the absorption and release of the reacted substances by negative pressure suction or positive pressure drainage.

[0052] The above implementation significantly reduces human intervention, improves the consistency and repeatability of sample processing, and is especially suitable for automated experimental platforms that operate continuously for long periods of time.

[0053] In an optional embodiment, the liquid suction mechanism 26 further includes a liquid storage tube 262 connected to the suction head 261. The suction head 261 is installed at the end of the liquid storage tube 262 through a detachable connection structure, which can be quickly installed and removed by means of snap-fit ​​or interference fit.

[0054] The aforementioned detachable connection method allows the aspiration mechanism 26 to replace the clean pipette tip 261 before each aspiration of the reacted substances from different reagent bottles 6, effectively avoiding cross-contamination between different samples and improving the accuracy and reliability of experimental results.

[0055] In an optional embodiment, the transfer device 2 further includes a fourth drive mechanism 25 to enable automated transfer of the reacted material from the reagent bottle 6 to the separation device 5.

[0056] like Figure 1 As shown, the fourth drive mechanism 25 is mounted on the second drive mechanism 22 and is arranged side-by-side with the third drive mechanism 23 on the same X-axis guide rail structure. Specifically, the second drive mechanism 22 not only drives the third drive mechanism 23 to move in the X direction, but also simultaneously drives the fourth drive mechanism 25 to run independently along the same X-axis guide rail. By setting independent motion coupling paths or using branch transmission mechanisms (such as dual slider modules or independent servo control), the fourth drive mechanism 25 can move independently relative to the third drive mechanism 23 in the X direction, avoiding mechanical interference and ensuring spatial coordination and motion accuracy when multiple tasks are executed in parallel.

[0057] Specifically, the second drive mechanism 22 also has a second X-axis drive motor, which drives the fourth drive mechanism 25 to slide along the X-axis guide rail via a synchronous belt, lead screw transmission or gear and rack transmission.

[0058] The aforementioned second X-axis drive motor can be an 86-stepper motor, with a positioning accuracy of ±0.2 mm.

[0059] In addition, the liquid suction mechanism 26 is connected to the fourth drive mechanism 25. The fourth drive mechanism 25 may include a Z-axis linear module, a pneumatic / electric push rod or a Z-axis drive motor. The Z-axis drive motor drives the liquid suction mechanism 26 to slide along the Z-axis guide rail through a synchronous belt or screw drive, so that the liquid suction mechanism 26 moves in the Z-axis.

[0060] To further automate the replacement of suction heads, such as Figure 9 As shown, in an optional embodiment, the automated high-throughput parallel synthesis and separation equipment for micro- and nano-copper powders also includes a pipette tip storage box 7 and a pipette tip replacement assembly 8, both of which are fixedly installed on the first platform 11 of the support 1.

[0061] Among them, such as Figure 9 As shown, the pipette tip storage box 7 has multiple vertically arranged receiving cavities. The receiving cavities are used to store clean pipette tips 71 to be picked up. The receiving cavities are arranged in an array, which makes it easy for the liquid suction mechanism 26 to move accurately along the X and Z directions and pick up the tips one by one under the drive of the fourth drive mechanism 25.

[0062] like Figure 9 As shown, the suction head replacement assembly 8 is located near the suction head storage box 7. It includes a frame 81 and a waste box 82. The frame 81 is provided with a scraping port 811. The scraping port 811 has an opening on the side and the size of the scraping port 811 is smaller than the outer diameter of the suction head 261.

[0063] When the suction mechanism 26 needs to remove the used suction head 261, the fourth drive mechanism 25 drives the liquid storage tube 262 to enter the suction port 811 horizontally from the opening on the side of the suction port 811. Then, the fourth drive mechanism 25 drives the liquid storage tube 262 to move upward in the vertical direction. Since the size of the suction port 811 is smaller than the outer diameter of the suction head 261, the suction head 261 will fall into the waste box 82 due to the obstruction of the frame 81. Then, the fourth drive mechanism 25 drives the liquid storage tube 262 to move upward and exit the suction port 811, move horizontally to the top of the suction head storage box 7, align with the new suction head 71 to be taken, and then move downward so that the liquid storage tube 262 is inserted into the suction head 71 to be taken, realizing the connection between the suction head 71 to be taken and the liquid storage tube 262.

[0064] The above-described implementation method enables automatic replacement of the suction head, improves the continuous operation capability of the equipment and the accuracy of the synthesis results, is suitable for multi-batch micro-nano material synthesis experiments, and facilitates the completion of the entire process without manual intervention, further enhancing the intelligence level and high-throughput processing advantages of the equipment.

[0065] The structure of the liquid preparation device 3 is described in detail below: In alternative implementations, such as Figure 2 and Figure 3 As shown, the liquid preparation device 3 includes a liquid supply mechanism 31, a rotating mechanism 32, and a sample inlet plate 33. The rotating mechanism 32 is mounted on the first platform 11, and the sample inlet plate 33 is connected to the rotating mechanism 32. The sample inlet plate 33 is provided with multiple supporting cavities 331 along the circumference for supporting each reagent bottle 6. The rotating mechanism 32 is configured to drive the sample inlet plate 33 to rotate. The liquid supply mechanism 31 is connected to the support 1 and has a liquid outlet end 3131 located above the sample inlet plate 33. The liquid outlet end 3131 is configured to sequentially supply reaction liquids with different ratios to each reagent bottle 6.

[0066] The sample inlet tray 33 is a circular or annular tray structure with multiple carrying cavities 331 evenly arranged along its circumference. Each carrying cavity 331 is used to accommodate one reagent bottle 6. The shape of the carrying cavity 331 is adapted to the outer wall of the reagent bottle 6, which can effectively fix the reagent bottle 6 and prevent it from tipping over or shifting during transportation or liquid supply.

[0067] by Figure 2 For example, the sample injection plate 33 is made of acrylic, with a diameter of 1000 mm and a thickness of 8 mm. The sample injection plate 33 has 24 carrying cavities 331 (diameter of 22.5 mm, suitable for 15 mL reagent bottles), which can hold 24 reagent bottles 6 of the solution to be mixed at the same time.

[0068] The rotating mechanism 32 is fixedly mounted on the first platform 11 via a flange and connected to the central axis of the sample inlet disk 33. It is configured to drive the sample inlet disk 33 to rotate intermittently around its central axis (the rotational speed can be 0~30 r / min). By controlling the rotation angle and step time, each bearing cavity 331 can be sequentially positioned below the liquid outlet 3131 of the liquid supply mechanism 31, thereby achieving sequential liquid supply. The rotating mechanism 32 can be driven by a stepper motor and a precision reducer to ensure precise and controllable rotation angle for each rotation, meeting the positional repeatability requirements in high-throughput experiments.

[0069] During use, the control unit can set the formula sequence of the reaction solution required for each reagent bottle 6 according to the preset experimental plan; after startup, the rotating mechanism 32 drives the sample inlet plate 33 to rotate, moving the reagent bottle 6 in the first carrier cavity 331 to directly below the liquid outlet 3131; the liquid supply mechanism 31 prepares the corresponding reaction solution according to the set first ratio and injects it into the reagent bottle 6 through the liquid outlet 3131; after completion, the sample inlet plate 33 rotates to the next station, and the liquid supply mechanism 31 prepares the corresponding reaction solution according to the set second ratio and injects it into the reagent bottle 6 through the liquid outlet 3131, and so on, until all reagent bottles 6 have been filled with liquid.

[0070] The above-described embodiment combines the rotary sample feeding disk 33 with the liquid supply mechanism 31 to achieve orderly distribution of reaction solutions with various ratios, thereby improving the flexibility and automation level of the liquid preparation process.

[0071] In an optional embodiment, the liquid supply mechanism 31 is used to precisely and controllably add reaction solutions of different proportions sequentially to multiple reagent bottles 6 to meet the high-throughput requirements of multi-component, multi-parameter reaction systems during the synthesis of micro / nano copper powder. For example... Figure 3 As shown, the liquid supply mechanism 31 includes a liquid storage component 311, a pump body component 312, and a liquid addition component 313.

[0072] Furthermore, the support 1 is provided with a first platform 11 and a second platform 12 arranged vertically. The first platform 11 is used to install the main functional modules such as the reaction device 4, the separation device 5, and the sample injection plate 33, while the second platform 12 is located below the first platform 11, forming a spatially layered layout, which is beneficial for the compactness of the equipment structure and the stability of the center of gravity. The liquid storage component 311 is fixedly installed on the second platform 12, making full use of the space under the equipment, avoiding the occupation of the operating area, and reducing the vibration impact of the overall equipment during operation.

[0073] The liquid storage assembly 311 includes multiple independently configured mother liquor storage containers, each used to hold a basic mother liquor, such as copper salt solution, reducing agent solution, dispersant solution, and ligand solution. These mother liquors are the basic raw materials for preparing the reaction solution required for the synthesis of micro / nano copper powder. Each storage container is connected to the pump assembly 312 via pipelines, and each pipeline can be equipped with an independent shut-off valve or solenoid valve to achieve independent control and on-demand supply of different mother liquors.

[0074] by Figure 1 and Figure 3 For example, the liquid storage assembly 311 consists of six 500 mL borosilicate glass reagent bottles (chemically resistant, with a light transmittance ≥90%, facilitating liquid level observation) and a 3D-printed ABS (Acrylonitrile Butadiene Styrene) plastic fixing frame. The fixing frame is secured to the second platform 12 using M6 fasteners, and the second platform 12 can be an aluminum profile desktop.

[0075] The pump assembly 312 is mounted on the support 1, for example, on a column on the side of the support 1. It includes multiple precision fluid delivery units, such as multi-channel peristaltic pumps, syringe pumps, or proportional diaphragm pumps, which can precisely control the extraction volume and mixing ratio of each mother liquor according to a preset program. The input end of each precision fluid delivery unit is connected to a mother liquor storage container in the liquid storage assembly 311, and the output end is connected to the input end of the liquid addition assembly 313, thereby delivering selected types and dosages of mother liquor sequentially or simultaneously to the liquid addition assembly 313 for mixing or direct distribution.

[0076] by Figure 3For example, pump assembly 312 includes six syringe pumps, all of which are commercially available high-precision syringe pumps (model can be Runze SY-09S, flow range 0.1 μL / min~10 mL / min, accuracy ±0.5%). Each syringe pump corresponds to one mother liquor storage container. The inlet of the syringe pump is connected to the mother liquor storage container via a PTFE tube (inner diameter 1 mm, temperature resistance -20℃~200℃), and the outlet is connected to the dispensing assembly 313 via a multi-port valve. The syringe pump has a built-in encoder, which can accurately measure the amount of mother liquor injected, adapting to the different formulation requirements for mother liquor volume (minimum adjustable volume 0.1 μL).

[0077] The liquid addition assembly 313 may include a mixing chamber and a fluid channel structure, and has multiple liquid inlets and a liquid outlet 3131. When a reaction solution with a specific formulation needs to be prepared, the pump assembly 312 injects different mother liquors into the liquid addition assembly 313 according to a set ratio. After uniform mixing in the mixing chamber, the mixture is then dripped into the reagent bottle 6 at the corresponding position in the sample inlet plate 33 via the liquid outlet 3131.

[0078] Specifically, the liquid filling assembly 313 is made of 3D-printed ABS with six 2 mm diameter through holes in the middle to hold six PTFE pipes in place.

[0079] The above-described implementation achieves efficient use of space by placing the liquid storage component 311 on the lower second platform 12; it uses the pump component 312 to accurately measure and controllably transport various mother liquors; and then uses the liquid addition component 313 to complete the preparation and targeted delivery of the final reaction liquid, thereby constructing an automated, modular, and high-precision liquid dispensing system, which significantly improves the flexibility and repeatability of the equipment in the synthesis of micro and nano materials.

[0080] The structure of reaction device 4 is described in detail below: In alternative implementations, such as Figure 4 As shown, the reaction apparatus 4 includes a heating and stirring assembly 41. Figure 4 As shown, the heating and stirring assembly 41 is equipped with a support platform, which has multiple reaction chambers 411 arranged in an array. Each reaction chamber 411 is adapted to accommodate a standard-sized reagent bottle 6. Below the support platform is a heating platform 412 (power 1500 W, temperature control range room temperature - 300℃, accuracy ±0.1℃). The heating platform 412 is an electric heating plate, ceramic heater, or other temperature-controllable heating element, configured to precisely control the temperature of the reagent bottle 6 in the support platform. The temperature range can be adjusted according to the requirements of the copper salt reduction reaction.

[0081] by Figure 4For example, the support platform has 36 reagent bottle holes (22 mm in diameter and 55 mm in depth) in a 6×6 pattern. The side openings of the support platform can extend deep into the platform. Temperature sensors are placed inside the holes, so that the heating platform 412 can control the temperature through a PID (Proportional-Integral-Derivative) temperature control module.

[0082] Furthermore, the heating and stirring assembly 41 also includes a magnetic field generator, which can be located below each reaction chamber 411 and integrated with or arranged in layers with the heating platform 412. The magnetic field generator is an electromagnetic coil array or a permanent magnet rotating mechanism, configured to generate an alternating or rotating magnetic field during operation to drive the stirring magnet placed in the reagent bottle 6 to rotate at high speed. The stirring rate can be adjusted by a program (0~1000 r / min) to achieve uniform mixing and enhanced mass transfer of the reaction solution. The magnetic field generator eliminates the need for a mechanical stirring shaft, avoiding sealing problems and the risk of cross-contamination, thus improving the reliability and cleanliness of the system.

[0083] To prevent copper powder from being oxidized by oxygen in the air at high temperatures, which would affect the purity and conductivity of the product, in an optional embodiment, the reaction apparatus 4 further includes a detachable or closable protective cover (not shown in the figure). The protective cover is entirely covered outside the heating and stirring assembly 41, forming a sealed reaction space. The protective cover is provided with an inlet (inner diameter of 6 mm) and an outlet (inner diameter of 8 mm). The inlet is connected to an external protective gas source via a gas pipeline. The protective gas is preferably an inert gas such as nitrogen (N2) or argon (Ar), and the flow rate of the protective gas can be controlled at 0~5 L / min by a solenoid valve. The outlet is connected to a tail gas treatment device, such as an activated carbon adsorption unit or a condensation recovery system, to collect and treat volatile byproducts or residual gases that may be released during the reaction.

[0084] In actual operation, a low-oxygen or even oxygen-free reaction atmosphere can be created by first introducing protective gas into the protective cover for a period of time to replace the internal air, and then starting the heating program.

[0085] In addition, the protective cover is an inverted U-shaped transparent cover (made of PC, impact resistant, light transmittance ≥85%), and the bottom of the cover is provided with a silicone sealing strip (thickness 5 mm, compression 3 mm), which can cover the heating and stirring component 41 to form a sealed space.

[0086] The protective cover can be rotatably connected to the heating and stirring assembly 41, and can be opened and closed by a telescopic mechanism such as a cylinder or hydraulic cylinder between the protective cover and the heating and stirring assembly 41; or the protective cover can be separately set from the heating and stirring assembly 41, and has a clamping end, which can be opened and closed by clamping and transferring by the first clamping mechanism 24.

[0087] In summary, the reaction apparatus 4 in the above embodiments not only achieves multi-channel synchronous heating and magnetic stirring, but also significantly improves the oxidation resistance and safety of the reaction process by introducing a protective cover and an inert atmosphere control system, making it particularly suitable for the batch synthesis of micro-nano powders of easily oxidized metal materials.

[0088] The structure of separation device 5 is described in detail below: In alternative implementations, such as Figure 5 As shown, the separation device 5 includes a plate 51 and a waste liquid tank 52. The plate 51 is provided with a plurality of separation holes 511, and a filter membrane is provided in the separation holes 511. The waste liquid tank 52 is sealed to the bottom end of the plate 51 and communicates with each separation hole 511. The waste liquid tank 52 has an air extraction port configured to communicate with the pump body.

[0089] by Figure 5 For example, plate 51 is a flat plate structure with certain rigidity and chemical stability, preferably made of transparent acrylic material, which facilitates observation of the liquid flow and filter membrane operation during the separation process. Multiple separation holes 511, penetrating the upper and lower surfaces, are arrayed on plate 51. Each separation hole 511 has a diameter of 25 mm, and the center-to-center distance between adjacent separation holes 511 is 15 mm, arranged in a 6×6 matrix, for a total of 36 separation holes 511. This layout design allows for the simultaneous parallel filtration of 36 samples in a single operation, significantly improving separation efficiency.

[0090] Each separation pore 511 contains a replaceable aqueous filter membrane, which is fixed to the inner wall of the pore 511. The membrane is preferably installed via an embedded slot or a thermostatic seal to ensure it does not shift or leak under negative pressure. The filter membrane has a pore size of 0.22 μm and can be made of hydrophilic materials such as polyethersulfone or mixed cellulose esters. It possesses excellent copper powder retention capacity and high throughput performance, effectively intercepting micro / nano copper powder particles larger than 0.22 μm while allowing the reaction mother liquor to pass through smoothly, achieving efficient solid-liquid separation.

[0091] The waste liquid tank 52 is located below the plate 51 and is sealed to the bottom surface of the plate 51, forming a closed negative pressure chamber. The main body of the waste liquid tank 52 is injection molded from high-density polyethylene material, with a volume of approximately 10 L. It has excellent resistance to acid and alkali corrosion and mechanical strength, making it suitable for waste liquid collection in various chemical systems. The top opening of the waste liquid tank 52 is completely fitted to the bottom of the plate 51, and an airtight connection is achieved through a 3 mm thick silicone sealing gasket to prevent air leakage during the filtration process and ensure stable system vacuum.

[0092] In addition, the internal space of the waste liquid tank 52 is connected to the lower outlet of the separation hole 511, allowing the liquid filtered by the filter membrane to flow into the waste liquid tank 52 for temporary storage under negative pressure. The waste liquid tank 52 has a drain port on its side wall, which is connected to an external waste liquid tank via a corrosion-resistant hose for periodically discharging the collected waste liquid. Furthermore, the waste liquid tank 52 also has an air extraction port located in the upper or top area of ​​the side wall, configured to connect to an external vacuum pump. When the vacuum pump is started, a negative pressure environment is created inside the waste liquid tank 52, with a pressure range adjustable from 0 to -0.09 MPa, thereby driving the reaction liquid to pass through the filter membrane from top to bottom into the waste liquid tank 52, completing rapid filtration.

[0093] The separation device 5 provided by the above embodiments is compact in structure, easy to operate, has high throughput, and is reliably sealed. It is particularly suitable for the post-processing stage in automated high-throughput micro-nano material synthesis systems and can effectively support the data accumulation and sample preparation needs of multi-parameter parallel experiments.

[0094] In alternative implementations, such as Figure 10 and Figure 11 As shown, the automated high-throughput parallel synthesis and separation equipment for micro- and nano-copper powders also includes a cooling device 011 and / or a sample rack 012; the cooling device 011 is installed on the first platform 11 and has multiple cooling chambers 0111 for placing each reagent bottle 6; the sample rack 012 is installed on the first platform 11 and has multiple sample slots 0121 for placing each reagent bottle 6 after the reaction.

[0095] Specifically, such as Figure 10 As shown, the cooling device 011 is located in the preset work station area of ​​the first platform 11 and is used to cool the reagent bottle 6 after the reaction. The cooling device 011 has multiple cooling chambers 0111 arranged in an array inside, and each cooling chamber 0111 is adapted to accommodate a standard size (e.g., 15 mL) reagent bottle 6 to ensure that the reagent bottle 6 can be placed stably and vertically.

[0096] The structure of the cooling device 011 can be the same as that of the reaction device 4. The difference is that the cooling device 011 does not have a heating platform 412 inside. It is cooled by metal heat conduction. During the cooling process, the reacted substances can be stirred by a magnetic field generator.

[0097] Additionally, the sample rack 012 is installed at a designated location on the first platform 11, typically downstream of the separation device 5 or in another area easily accessible by the transfer device 2, for storing the reagent bottles 6 after the reaction. Figure 11 As shown, the sample rack 012 has multiple sample slots 0121 arranged in a regular array. Each sample slot 0121 can hold a reagent bottle 6, thus realizing the orderly placement of multiple samples.

[0098] After the entire automated process is completed, the user can retrieve all reagent bottles 6 at once through sample rack 012 for centralized processing.

[0099] In an optional embodiment, the automated high-throughput parallel synthesis and separation equipment for micro- and nano-copper powders also includes a control unit, and the transfer device 2, the liquid preparation device 3, the reaction device 4, and the separation device 5 are all connected to the control unit.

[0100] The control unit can use an industrial-grade PLC (model S7-1200) as the main controller, and connect to various drive mechanisms, 6 injection pumps, heating and stirring assembly 41, solenoid valve for controlling protective airflow, vacuum pump, etc. via the 485 communication protocol; at the same time, the PLC connects to the Arduino development board via USB to control the opening, closing and rotation of the first clamping mechanism 24 and the second clamping mechanism 9, as well as the data acquisition of the liquid level sensor, temperature sensor and torque sensor (sampling frequency 10 Hz).

[0101] The aforementioned control unit can be used in conjunction with a software system written in Python, running on Windows 10, and has the following functions: Parameter settings: Supports filling in the test plan (including mother liquor type, amount of mother liquor injected per bottle, reaction temperature, reaction time, stirring speed, nitrogen flow rate, and vacuum degree of filtration) in an Excel spreadsheet. The software automatically reads and parses the data in the spreadsheet. Automatic execution: The software automatically executes the process of "disc sample injection → mother liquor injection → mixing → transfer to reaction device → nitrogen protection → heating and stirring reaction → transfer to separation device → filtration separation → sample storage → waste disposal" without manual intervention.

[0102] The following is a specific example illustrating the use of the above-mentioned automated high-throughput parallel synthesis and separation equipment for micro / nano copper powder: 1. Place copper sulfate solution (CuSO4·5H2O: 25 g prepared into 150 mL solution), sodium chloride solution (NaCl: 1.5 g prepared into 150 mL solution), triethanolamine solution (triethanolamine: 20 g, prepared into 150 mL solution), ascorbic acid solution (ascorbic acid: 28 g, NaOH: 6.6 g), PVP solution (PVP: 3 g), and water into six mother liquor storage containers, respectively. Place 24 clean 15 mL reagent bottles 6 evenly on the sample loading tray 33; check the gripping accuracy of the first clamping mechanism 24 and the second clamping mechanism 9, ensuring that the liquid aspiration mechanism 26 and the liquid addition assembly 313 are unblocked, and that the temperature control and vacuum systems of the heating and stirring assembly 41 and the separation device 5 are functioning normally.

[0103] 2. Test plan and parameter settings: In the software system supporting the device, the mother liquor volume parameters of 24 groups of experimental formulations are entered through an Excel table. As shown in Table 1, they are the proportioning data of 24 groups of reaction solutions, and the reaction and separation parameters are uniformly set: reaction temperature: 85 °C; stirring speed: 600 r / min; reaction time: 180 min; nitrogen flow rate: 1.5 L / min (continuously introduced to prevent copper powder oxidation); suction filtration vacuum degree: 0.075 MPa; Liquid injection accuracy: Guaranteed by an injection pump, with a volume error ≤ ±0.01 mL.

[0104] Table 1

[0105] 3. Automated synthesis and separation process: After starting the device, the system automatically executes the entire process of "liquid mixing → high-temperature reaction → solid-liquid separation → sample storage" without manual intervention. The following are the descriptions of the key steps: Precise mixing of mother liquor (taking the first group of formulations as an example) The system reads the first group of formulations: stock solution A 1.0 mL, stock solution B 0.5 mL, stock solution C 1.0 mL, stock solution D 5.5 mL, stock solution E 1.0 mL, stock solution F 5.0 mL (total liquid volume 14.0 mL).

[0106] The liquid addition component 313 is located above the sampling tray 33. Six injection pumps are started synchronously, and the corresponding stock solutions are extracted according to the set volume, and injected synchronously through a tetrafluoroethylene tube; after the liquid injection is completed, the first clamping mechanism 24 sequentially grabs the reagent bottles after mixing the liquids and transfers them to the 36 reaction holes of the heating and stirring component 41; at the same time, the rotating mechanism 32 drives the sampling tray 33 to rotate to the next reagent bottle for sampling.

[0107] The protective cover descends and covers above the heating and stirring component 41 to form a sealed space, and nitrogen is continuously introduced at a flow rate of 1.5 L / min to displace the air in the space; The heating table 412 is heated to 85 °C (PID temperature control accuracy ±0.1 °C), and at the same time, magnetic stirring is started (stirring speed 600 r / min). Each reaction chamber 411 independently controls the temperature and speed to ensure that the 24 groups of formulations react for 180 min under the set conditions, realizing the uniform reduction of copper ions and the growth of copper powder.

[0108] 4. High-efficiency solid-liquid separation After the reaction ends: The second clamping mechanism 9 cooperates with the first clamping mechanism 24 to loosen the bottle cap of the reagent bottle; The liquid suction mechanism 26 aspirates the solution after the reaction and transfers it to the separation hole 511, aligning the solution with the filtration hole. The vacuum pump is started, and under a vacuum of 0.075 MPa, the reaction waste liquid quickly permeates into the waste liquid tank 52 through a 0.22 μm aqueous filter membrane, while the micro-nano copper powder is retained on the surface of the filter membrane. The filtration process of 24 samples in a single batch is completed simultaneously, taking ≤5 min, which greatly improves the separation efficiency.

[0109] 5. Product performance verification: The particle size distribution, morphology, and purity of the 24 experimentally synthesized micro / nano copper powders were detected using scanning electron microscopy. Figure 12 SEM images of the micro / nano copper powders synthesized in 24 experimental groups are shown. The results indicate that the copper powders in each group have a uniform particle size distribution, with a median diameter in the range of 100 nm to 200 nm. The morphology is mainly spherical, with good dispersibility and no obvious agglomeration.

[0110] Through the above-described structure and process setup, this embodiment completes the synthesis and separation of micro / nano copper powder under multiple different reaction parameter conditions within the same operating cycle, avoiding systematic errors caused by manual operation and verifying the engineering applicability of the equipment in high-throughput process exploration scenarios. In the above process, each reagent bottle operates along an independent processing path from solution preparation to separation, avoiding cross-interference between different reaction systems from a structural and process perspective.

[0111] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. An automated high-throughput parallel synthesis and separation device for micro / nano copper powder, comprising a support (1), a transfer device (2), a liquid preparation device (3), a reaction device (4), and a separation device (5), characterized in that: The support (1) has a first platform (11), at least a portion of the structure of the liquid preparation device (3), the reaction device (4) and the separation device (5) are mounted on the first platform (11). The solution preparation device (3) is configured to carry multiple reagent bottles (6) and sequentially supply reaction solutions with different ratios to each of the reagent bottles (6); The reaction device (4) is provided with multiple reaction chambers (411), each of which is used to provide an independent reaction environment for the corresponding reagent bottle (6); The separation device (5) is provided with multiple separation holes (511), and each separation hole (511) and the reaction chamber (411) are in a one-to-one correspondence in terms of quantity and spatial position, for independent solid-liquid separation of the reacted substances in each reagent bottle (6); The transfer device (2) is connected to the support (1) and located above the first platform (11). The transfer device (2) is configured to transfer the reagent bottle (6) along the X, Y and Z directions, and sequentially complete the transfer operation of the reagent bottle (6) between the liquid preparation device (3), the reaction device (4) and the separation device (5) according to the preset running path.

2. The automated high-throughput parallel synthesis and separation equipment for micro / nano copper powder according to claim 1, characterized in that, The transfer device (2) includes a first drive mechanism (21), a second drive mechanism (22), a third drive mechanism (23), and a first clamping mechanism (24). The first drive mechanism (21) is mounted on the bracket (1) and connected to the second drive mechanism (22). The first drive mechanism (21) is configured to drive the second drive mechanism (22) to move along the Y direction. The second drive mechanism (22) is connected to the third drive mechanism (23), and the second drive mechanism (22) is configured to drive the third drive mechanism (23) to move along the X direction; The third driving mechanism (23) is connected to the first clamping mechanism (24). The third driving mechanism (23) is configured to drive the first clamping mechanism (24) to move along the Z direction. The first clamping mechanism (24) is configured to pick up, place and rotate the reagent bottle (6).

3. The automated high-throughput parallel synthesis and separation equipment for micro / nano copper powder according to claim 2, characterized in that, The transfer device (2) also includes a liquid suction mechanism (26); The liquid aspiration mechanism (26) is detachably connected to a pipette tip (261) for aspirating the reacted substance in the reagent bottle (6). The liquid aspiration mechanism (26) transfers the reacted substance in each of the reagent bottles (6) through the pipette tip (261). When transferring between different reagent bottles (6), the pipette tip (261) can be replaced to achieve physical isolation between different reaction systems.

4. The automated high-throughput parallel synthesis and separation equipment for micro / nano copper powder according to claim 3, characterized in that, The transfer device (2) also includes a fourth drive mechanism (25); The fourth drive mechanism (25) is connected to the second drive mechanism (22), and the second drive mechanism (22) is further configured to drive the fourth drive mechanism (25) to move independently of the third drive mechanism (23) along the X direction; The fourth driving mechanism (25) is connected to the liquid suction mechanism (26). The fourth driving mechanism (25) is configured to drive the liquid suction mechanism (26) to move along the Z direction. The liquid suction mechanism (26) is configured to transfer the reacted substance in the reagent bottle (6) to the separation device (5).

5. The automated high-throughput parallel synthesis and separation equipment for micro / nano copper powder according to claim 3, characterized in that, The automated high-throughput parallel synthesis and separation equipment for micro- and nano-copper powder also includes a pipette tip storage box (7) and a pipette tip replacement assembly (8) both installed on the first platform (11). The pipette tip storage box (7) stores a plurality of vertically placed pipette tips (71) to be taken. The pipette tip replacement assembly (8) has a rejection port (811) for rejecting the pipette tips (261) on the liquid suction mechanism (26) and a waste box (82) located below the rejection port (811).

6. The automated high-throughput parallel synthesis and separation equipment for micro / nano copper powder according to claim 2, characterized in that, It also includes a second clamping mechanism (9) and a screw cap structure (10) both mounted on the first platform (11). The screw cap structure (10) is provided with a limiting cavity (101) for accommodating the reagent bottle (6), and the second clamping mechanism (9) is used to clamp the body of the reagent bottle (6).

7. The automated high-throughput parallel synthesis and separation equipment for micro / nano copper powder according to claim 1, characterized in that, The liquid preparation device (3) includes a liquid supply mechanism (31), a rotating mechanism (32), and a sample inlet plate (33). The rotating mechanism (32) is installed on the first platform (11), the sample inlet disk (33) is connected to the rotating mechanism (32), the sample inlet disk (33) is provided with multiple bearing cavities (331) along the circumferential direction for bearing each of the reagent bottles (6), and the rotating mechanism (32) is configured to drive the sample inlet disk (33) to rotate.

8. The automated high-throughput parallel synthesis and separation equipment for micro / nano copper powder according to claim 7, characterized in that, The liquid supply mechanism (31) is connected to the support (1) and has a liquid outlet (3131) located above the sample inlet plate (33). The liquid outlet (3131) is configured to supply reaction liquids with different ratios to each of the reagent bottles (6) in sequence.

9. The automated high-throughput parallel synthesis and separation equipment for micro / nano copper powder according to claim 7, characterized in that, The liquid supply mechanism (31) includes a liquid storage component (311), a pump body component (312), and a liquid addition component (313). The support (1) has a second platform (12) located below the first platform (11), and the liquid storage assembly (311) is installed on the second platform (12). The liquid storage assembly (311) is used to store multiple mother liquors. The pump assembly (312) and the liquid filling assembly (313) are both mounted on the bracket (1). The pump assembly (312) is connected between the liquid storage assembly (311) and the liquid filling assembly (313). The pump assembly (312) is configured to pump each of the mother liquors in the liquid storage assembly (311) into the liquid filling assembly (313).

10. The automated high-throughput parallel synthesis and separation equipment for micro / nano copper powder according to claim 1, characterized in that, The reaction apparatus (4) includes a heating and stirring assembly (41) and a protective cover; The heating and stirring assembly (41) includes multiple reaction chambers (411), a magnetic field generator, and a heating platform (412) located below the reaction chambers (411). The protective cover is configured to cover the heating and stirring assembly (41), and the protective cover has an air inlet configured to communicate with a protective gas source and an air outlet configured to communicate with an exhaust gas treatment device.

11. The automated high-throughput parallel synthesis and separation equipment for micro / nano copper powder according to claim 1, characterized in that, The separation device (5) includes a plate (51) and a waste liquid tank (52); The plate (51) is provided with a plurality of separation holes (511), and a filter membrane is provided in the separation holes (511); The waste liquid tank (52) is sealed to the bottom end of the plate (51) and communicates with each of the separation holes (511). The waste liquid tank (52) has an air extraction port configured to communicate with the pump body.

12. The automated high-throughput parallel synthesis and separation equipment for micro / nano copper powder according to any one of claims 1 to 9, characterized in that, It also includes a cooling device (011) and / or a sample holder (012); The cooling device (011) is installed on the first platform (11), and the cooling device (011) is provided with multiple cooling chambers (0111) for placing each of the reagent bottles (6). The sample rack (012) is installed on the first platform (11), and the sample rack (012) is provided with multiple sample slots (0121) for placing each of the reagent bottles (6) after the reaction.

13. The automated high-throughput parallel synthesis and separation equipment for micro / nano copper powder according to any one of claims 1 to 9, characterized in that, It also includes a control unit, and the transfer device (2), the liquid preparation device (3), the reaction device (4) and the separation device (5) are all connected to the control unit.

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