A liquid phase laser ablation mass production device

Abstract

This utility model discloses a large-scale production device for liquid phase laser ablation, including a laser generating mechanism, a liquid phase ablation reaction mechanism, a slurry storage device, a catalyst slurry storage device, a monitoring mechanism, and a controller. The laser generating mechanism outputs laser light into the liquid phase ablation reaction mechanism. The liquid phase ablation reaction mechanism includes a light-blocking black box, a reaction chamber, and a temperature control mechanism. The reaction chamber is located inside the light-blocking black box, which allows the laser to irradiate into the reaction chamber. The input end of the reaction chamber is connected to the slurry storage device in a controllable manner, and the output end of the reaction chamber is connected to the catalyst slurry storage device in a controllable manner. The temperature control mechanism regulates the temperature within the reaction chamber. The monitoring mechanism monitors the reaction parameters of the large-scale production device for liquid phase laser ablation. The controller adjusts the operating parameters based on the monitoring results, thereby solving the problem of the difficulty in achieving large-scale production in the prior art.

Description

Technical Field

[0001] This utility model relates to the technical field of equipment for preparing nanocatalytic materials, and in particular to a liquid phase laser ablation mass production device. Background Technology

[0002] In the water electrolysis hydrogen production industrial system, high-performance catalysts are considered the "heart" of the entire process, playing an irreplaceable and crucial role. Their efficiency directly determines the efficiency and cost of hydrogen energy conversion. Highly efficient catalysts can produce more hydrogen with the same electrical input, greatly improving energy utilization efficiency; simultaneously, they reduce energy consumption during the reaction process, thereby lowering hydrogen production costs, which is of great significance for promoting the commercialization of the "green hydrogen" industry. However, mainstream catalysts, represented by platinum and iridium, are extremely scarce in nature, and their extraction and purification are difficult, resulting in persistently high market prices. These factors severely restrict the large-scale application of "green hydrogen" technology, making it difficult to reduce the production cost of "green hydrogen" and hindering its effective competition with traditional fossil fuel-based hydrogen production in the market, thus impeding the rapid development of the entire hydrogen energy industry.

[0003] Therefore, the development of novel catalysts and their preparation technologies that are efficient, low-cost, and easy to scale up is urgently needed and has increasingly become a focus of attention in the industry. However, the current development of novel catalysts faces multiple challenges. From the perspective of preparation processes, traditional methods generally suffer from high energy consumption and heavy pollution. The production process requires a large amount of energy and resources, while generating pollutants such as wastewater and waste gas, which contradicts the green and environmentally friendly concept of "green hydrogen." Furthermore, traditional processes face numerous difficulties in scaling up production, making it difficult to achieve rapid increases in output and effective cost control. In addition, novel catalysts also face the problem of being disconnected from electrode preparation technology and having low integration in practical applications. This makes it difficult for the catalyst to fully realize its performance advantages, affecting the overall efficiency and stability of the water electrolysis hydrogen production system, further increasing the difficulty of moving novel catalysts from the laboratory to industrial applications. Utility Model Content

[0004] The purpose of this invention is to provide a liquid phase laser ablation mass production device to solve the problem that existing technologies cannot achieve integrated and large-scale production of catalyst and membrane electrode manufacturing.

[0005] To address the aforementioned technical problems, this utility model provides a large-scale production device for liquid-phase laser ablation, comprising a laser generating mechanism, a liquid-phase ablation reaction mechanism, a slurry storage device, a catalyst slurry storage device, a monitoring mechanism, and a controller. The laser generating mechanism outputs laser light into the liquid-phase ablation reaction mechanism. The liquid-phase ablation reaction mechanism includes a light-blocking black box, a reaction chamber, and a temperature control mechanism. The reaction chamber is located inside the light-blocking black box, which allows laser light to irradiate the reaction chamber. The input end of the reaction chamber is connected to the slurry storage device in a controllable manner, and the output end of the reaction chamber is connected to the catalyst slurry storage device in a controllable manner. The temperature control mechanism regulates the temperature within the reaction chamber. The monitoring mechanism monitors the reaction parameters of the large-scale liquid-phase laser ablation production device. The controller regulates the operating parameters of the large-scale liquid-phase laser ablation production device based on the monitoring results.

[0006] In one embodiment, the laser generating mechanism includes a laser, a high lens, a beam expander, a galvanometer, and a focusing field lens arranged sequentially along the laser delivery optical path. The focusing field lens is disposed on the light-blocking black box and is aligned with the liquid phase melting reaction mechanism.

[0007] In one embodiment, the monitoring mechanism includes a laser energy meter for detecting laser energy information at the high lens and sending it to the controller.

[0008] In one embodiment, the light-blocking black box is equipped with a three-dimensional displacement platform, and the reaction chamber is located on the three-dimensional displacement platform.

[0009] In one embodiment, the temperature control mechanism includes a cooling circulation base and a temperature controller. The reaction chamber is provided on the cooling circulation base, and the temperature controller is used to regulate the cooling temperature of the cooling circulation base.

[0010] In one embodiment, a feed pump is connected between the output of the slurry temporary storage device and the input of the reaction chamber.

[0011] In one embodiment, the input terminal of the slurry temporary storage device is connected in parallel to a first feed switch and a second feed switch; the first feed switch is used for direct feeding; the second feed switch is connected to a slurry mixer, which is used for mixing and distributing different materials.

[0012] In one embodiment, a discharge pump is connected between the input end of the catalyst slurry temporary storage device and the output end of the reaction chamber.

[0013] In one embodiment, the monitoring mechanism includes a thermocouple and a temperature monitor; the thermocouple is disposed on the reaction chamber and is used to detect the internal temperature of the reaction chamber; the temperature monitor is used to send the detection result of the thermocouple to the controller.

[0014] The beneficial effects of this utility model are as follows:

[0015] It has fewer steps, shorter time consumption, and higher integration, enabling continuous production and obtaining catalyst slurry that can be used for subsequent membrane electrode preparation in one step. Furthermore, the solid content of the slurry is continuously adjustable, and the catalyst slurry is temporarily stored in a catalyst slurry temporary storage device, which facilitates the integrated preparation of the catalyst and membrane electrode.

[0016] The breakthrough direction of this equipment technology is to develop a macro-quantitative LAL device that integrates laser energy regulation, slurry circulation cooling, and online monitoring, so as to realize continuous, low-energy-consumption, and zero-pollution production of catalyst slurry, and directly adapt to the membrane electrode preparation process. Attached Figure Description

[0017] To more clearly illustrate the technical solution of this utility model, the drawings used in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this utility model. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0018] Figure 1 This is a structural schematic diagram provided by an embodiment of the present utility model.

[0019] The attached figures are labeled as follows:

[0020] 10. Laser generating mechanism; 11. Laser; 12. High lens; 13. Beam expander; 14. Galvanometer; 15. Focusing field lens;

[0021] 20. Liquid phase melting reaction mechanism; 21. Light-blocking black box; 22. Reaction chamber; 23. Temperature control mechanism; 231. Cooling circulation base; 232. Temperature controller;

[0022] 30. Slurry temporary storage device; 31. Feed pump; 321. First feed switch; 322. Second feed switch; 33. Slurry mixer;

[0023] 40. Catalyst slurry temporary storage device; 41. Discharge pump;

[0024] 50. Monitoring agency; 51. Laser energy meter; 52. Thermocouple; 53. Temperature monitor;

[0025] 60. Controller;

[0026] 70. Slurry flow channel. Detailed Implementation

[0027] The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments.

[0028] This invention provides a liquid phase laser ablation macro-quantity production device, the implementation of which is as follows: Figure 1 As shown, it includes a laser generating mechanism 10, a liquid phase ablation reaction mechanism 20, a slurry temporary storage device 30, a catalyst slurry temporary storage device 40, a monitoring mechanism 50, and a controller 60.

[0029] Regarding the laser generating mechanism 10, it is used to output laser light into the liquid phase melting reaction mechanism 20, such as... Figure 1 As shown, in this embodiment, the laser generating mechanism 10 includes a laser 11, a high lens 12, a beam expander 13, a galvanometer 14, and a focusing field lens 15 arranged sequentially along the laser transmission optical path. The focusing field lens 15 is mounted on the light-blocking black box 21 of the liquid phase melting reaction mechanism 20, and the focusing field lens 15 is aligned with the liquid phase melting reaction mechanism 20.

[0030] The laser 11 can be a nanosecond or picosecond laser. When a nanosecond laser is used, its repetition frequency is 10–100 Hz and its single pulse energy is 100–1000 mJ. When a picosecond laser is used, its repetition frequency is 1000–3000 Hz and its single pulse energy is 100–500 μJ. The high-transmittance lens 12 can be selected as a high-transmittance optical element with a transmittance of 98%. The scanning range of the galvanometer 14 can be set to 50*50 cm. The focal length of the focusing field lens 15 can be set to 500–1000 mm.

[0031] After adopting the above configuration, the laser emitted by the laser 11 can be transmitted to the beam expander 13 through the high lens 12. After passing through the beam expander 13, the laser acts on the galvanometer 14. The galvanometer 14 reflects and transmits all the energy to the focusing field lens 15, and the focusing field lens 15 focuses the laser into the liquid phase melting reaction mechanism 20, thereby providing the necessary energy for the reaction.

[0032] Regarding the liquid phase melting reaction mechanism 20, such as Figure 1 As shown, this embodiment sets the liquid phase melting reaction mechanism 20 to include a light-blocking black box 21, a reaction chamber 22, and a temperature control mechanism 23.

[0033] For the light-blocking black box 21, such as Figure 1As shown, in this embodiment, the interior of the light-blocking black box 21 is equipped with a reaction chamber 22. The light-blocking black box 21 is used to allow laser irradiation into the reaction chamber 22, thereby enabling the light-blocking black box 21 to provide a sealed light-blocking environment for the reaction chamber 22 to ensure the stable progress of the reaction.

[0034] In this embodiment, a three-dimensional displacement platform is provided inside the light-blocking black box 21, and a reaction chamber 22 is provided on the three-dimensional displacement platform.

[0035] After adopting the above configuration, the three-dimensional displacement platform can drive the reaction cavity 22 to move in three directions (XYZ). At this time, by controlling the movement of the reaction cavity 22 through the three-dimensional displacement platform, it can work in conjunction with the focusing field lens 15, so that the high-energy laser beam can perform serpentine or circular scanning within the reaction cavity 22, ensuring that the reaction cavity 22 can obtain the appropriate laser energy density at each position.

[0036] The reaction chamber 22 is the site where the reaction takes place, such as... Figure 1 As shown, in this embodiment, the bottom of the reaction chamber 22 is equipped with a stirring device and a fixed position for the solid target material. The input end of the reaction chamber 22 is connected to the slurry storage tank 30 in a controllable manner, and the output end of the reaction chamber 22 is connected to the catalyst slurry storage tank 40 in a controllable manner. For example, corresponding valves can be set at the input and output ends of the reaction chamber 22. By controlling the opening and closing states of the valves at both ends, the input, residence, and output of the slurry into the reaction chamber 22 can be realized.

[0037] It should be noted that this embodiment also sets the reaction chamber 22 as a detachable and replaceable structure so that different sizes of reaction chamber 22 can be replaced according to different reaction requirements. For example, the reaction chamber 22 can be set to have multiple size options within 20ml to 1L, specifically reaction liners of 20ml, 50ml, 100ml, 200ml, 500ml, 800ml and 1L.

[0038] The temperature control mechanism 23 is used to regulate the temperature inside the reaction chamber 22, such as... Figure 1 As shown, in this embodiment, the temperature control mechanism 23 includes a cooling circulation base 231 and a temperature controller 232. The cooling circulation base 231 is provided with a reaction chamber 22, and the temperature controller 232 is used to regulate the cooling temperature of the cooling circulation base 231.

[0039] Specifically, the cooling circulation base 231 can be placed on a three-dimensional displacement platform, and the reaction chamber 22 can be detachably and replaceably placed on the cooling circulation base 231. Therefore, the reaction chamber 22 can not only maintain the function of movement and detachment and replacement, but also exchange heat with the cooling circulation base 231.

[0040] For example, the temperature controller 232 can control the circulation of cooling liquid inside the cooling circulation base 231. Therefore, when the reaction chamber 22 generates high temperature due to the reaction, the cooling circulation base 231 can cool the reaction chamber 22 in a timely manner.

[0041] The cooling liquid can be pumped into the cooling circulation base 231 by a corresponding pump for circulation. Therefore, the temperature controller 232 can regulate the cooling efficiency of the cooling circulation base 231 by adjusting the operating efficiency of the corresponding pump. The temperature reference data regulated by the temperature controller 232 can be obtained by the monitoring mechanism 50. Therefore, after adopting the above setting method, the temperature control mechanism 23 can achieve precise temperature control from -196 to 80℃, with a temperature control accuracy of less than 0.2℃.

[0042] In addition, such as Figure 1 As shown, both the slurry temporary storage unit 30 and the catalyst slurry temporary storage unit 40 are connected to the inside of the reaction chamber 22 via the slurry flow channel 70. Therefore, the slurry flow channels 70 of both can be integrated into the inside of the cooling circulation base 231, which can not only improve the overall structural compactness of the equipment, but also realize the circulation cooling of the slurry.

[0043] Regarding the slurry storage device 30, its main function is to temporarily store the slurry and transport it into the reaction chamber 22, such as... Figure 1 As shown, in this embodiment, a feed pump 31 is connected between the output end of the slurry temporary storage 30 and the input end of the reaction chamber 22. With the above configuration, as long as the feed pump 31 is started, the slurry in the slurry temporary storage 30 can be transported into the reaction chamber 22.

[0044] The slurry temporary storage device 30 has two different application modes, specifically as follows: Figure 1 As shown, in this embodiment, the input terminal of the slurry temporary storage device 30 is connected to a first feed switch 321 and a second feed switch 322. The first feed switch 321 is used for direct feeding. The second feed switch 322 is connected to a slurry mixer 33, which is used for mixing and outputting different materials.

[0045] After adopting the above setup, the slurry that is ready to use can be stored in the slurry temporary storage 30 through the first feed switch 321 and then fed into the reaction chamber 22 for reaction. The slurry that needs to be mixed can be sent to the slurry mixer 33 for mixing first. After the slurry is fully mixed, the second feed switch 322 is opened and the mixed slurry is sent to the slurry temporary storage 30 and then sent into the reaction chamber 22 for reaction.

[0046] Regarding the catalyst slurry temporary storage device 40, its main purpose is to temporarily store the slurry after the reaction, such as... Figure 1 As shown, in this embodiment, a discharge pump 41 is connected between the input end of the catalyst slurry temporary storage device 40 and the output end of the reaction chamber 22. With the above configuration, as long as the discharge pump 41 is started, the slurry in the reaction chamber 22 can be transported and stored to the catalyst slurry temporary storage device 40.

[0047] Regarding the monitoring agency 50, it is used to monitor the reaction parameters of the liquid phase laser ablation mass production unit, such as... Figure 1 As shown, in this embodiment, the monitoring mechanism 50 includes a laser energy meter 51, a thermocouple 52, and a temperature monitor 53. The laser energy meter 51 is used to detect the laser energy information at the high lens 12 and send it to the controller 60. The thermocouple 52 is disposed on the reaction chamber 22 and is used to detect the internal temperature of the reaction chamber 22. The temperature monitor 53 is used to send the detection result of the thermocouple 52 to the controller 60.

[0048] After adopting the above configuration, the laser energy meter 51 can collect energy from the high lens 12 for monitoring. For example, in this embodiment, 2% reflected light is collected from the high lens 12 for energy monitoring, and the measured laser energy information is sent to the controller 60. The cooperation between the thermocouple 52 and the temperature monitor 53 can realize real-time monitoring of the temperature inside the reaction chamber 22, thereby facilitating the controller 60 to perform subsequent automated control processing.

[0049] Regarding the controller 60, it is used to adjust the operating parameters of the liquid phase laser ablation mass production device according to the monitoring results. For example, the controller 60 can control the temperature of the reaction slurry in the reaction chamber 22 by setting the temperature monitor 53 in real time according to the temperature fluctuation.

[0050] During application, the laser generating mechanism 10 emits a laser beam that meets the requirements and enters the reaction chamber 22 inside the light-blocking black box 21. Since the slurry storage device 30 inputs the slurry to be reacted into the reaction chamber 22, and the temperature control device 23 controls the reaction temperature, the reaction chamber 22 will react in a preset manner. The catalyst generated after the reaction will be output to the catalyst slurry storage device 40 for storage. The monitoring device 50 will monitor the entire process in real time to ensure that the controller 60 can make corresponding adjustments in a timely manner, thus realizing the continuous production of catalyst slurry.

[0051] To provide a more detailed description of the liquid phase laser ablation mass production apparatus of this embodiment, the following will illustrate it in conjunction with two specific applications:

[0052] Application Method 1: Production of low-platinum electrolytic water production hydrogen cathode catalyst

[0053] A precursor of 99.9% high-purity platinum powder / carbon nanotubes at a mass ratio of 1:9 and a mixed solvent of isopropanol / water at a volume ratio of 1:1 are premixed in a slurry mixer 33 and then pumped into a reaction chamber 22 with a volume of 1L. A platinum metal target with a diameter of 12cm and a thickness of 3mm is fixed at the bottom of the reaction chamber 22. The temperature of the temperature control mechanism 23 is set to 10℃. The nanosecond laser is turned on, and the energy of the laser 11 is set to 1000mJ and the repetition frequency is set to 100Hz. The high-energy laser beam is controlled by the galvanometer 14 to perform a 10cm diameter ring scanning laser action on the reaction slurry in the reaction chamber 22. After 1 hour of laser action, a low-platinum electrolysis water-to-hydrogen catalyst slurry can be obtained.

[0054] Application Method 2: Production of Low-Iridium Electrolytic Water Hydrogen Production Anode Catalyst

[0055] A precursor of 99.9% high-purity iridium powder / titanium oxide (TiO2) at a mass ratio of 1:9 and a mixed solvent of isopropanol / water at a volume ratio of 2:1 were premixed in a slurry mixer 33 and pumped into a reaction chamber 22 with a volume of 500 ml. The temperature of the temperature control mechanism 23 was set to -60℃. The picosecond laser was turned on, and the energy of the laser 11 was set to 300 μJ and the repetition frequency was set to 2000 Hz. The high-energy laser beam was controlled by the galvanometer 14 to perform serpentine scanning laser action on the reaction slurry in the reaction chamber 22. The scanning area was 6*6 cm. After 20 minutes of laser action, a low-iridium electrolytic water electrolysis hydrogen production anode catalyst slurry was obtained.

[0056] The above description is the preferred embodiment of this utility model. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of this utility model, and these improvements and modifications are also considered to be within the protection scope of this utility model.

Claims

1. A liquid phase laser ablation mass production device, characterized in that, It includes a laser generating mechanism, a liquid phase ablation reaction mechanism, a slurry storage device, a catalyst slurry storage device, a monitoring mechanism, and a controller; The laser generating mechanism is used to output laser light into the liquid phase melting reaction mechanism; The liquid phase melting reaction mechanism includes a light-blocking black box, a reaction chamber, and a temperature control mechanism; the reaction chamber is located inside the light-blocking black box, and the light-blocking black box is used to allow laser irradiation into the reaction chamber; the input end of the reaction chamber is connected to the slurry temporary storage device in a controllable manner, and the output end of the reaction chamber is connected to the catalyst slurry temporary storage device in a controllable manner. The temperature control mechanism is used to regulate the temperature inside the reaction chamber; The monitoring mechanism is used to monitor the reaction parameters of the liquid phase laser ablation macro-quantitative production device. The controller is used to adjust the operating parameters of the liquid phase laser ablation mass production device based on the monitoring results.

2. The liquid phase laser ablation macro-quantization production device according to claim 1, characterized in that, The laser generating mechanism includes a laser, a high lens, a beam expander, a galvanometer, and a focusing field lens arranged sequentially along the laser delivery optical path. The focusing field lens is mounted on the light-blocking black box and is aligned with the liquid phase melting reaction mechanism.

3. The liquid phase laser ablation macro-quantization production apparatus according to claim 2, characterized in that, The monitoring mechanism includes a laser energy meter, which is used to detect the laser energy information at the high lens and send it to the controller.

4. The liquid phase laser ablation macro-quantization production apparatus according to claim 1, characterized in that, The light-blocking black box is equipped with a three-dimensional displacement platform, and the reaction chamber is located on the three-dimensional displacement platform.

5. The liquid phase laser ablation macro-quantity production apparatus according to claim 1, characterized in that, The temperature control mechanism includes a cooling circulation base and a temperature controller. The reaction chamber is provided on the cooling circulation base, and the temperature controller is used to regulate the cooling temperature of the cooling circulation base.

6. The liquid phase laser ablation macro-quantization production apparatus according to claim 1, characterized in that, A feed pump is connected between the output end of the slurry temporary storage device and the input end of the reaction chamber.

7. The liquid phase laser ablation macro-quantization production apparatus according to claim 6, characterized in that, The input terminal of the slurry temporary storage device is connected in parallel to a first feed switch and a second feed switch; The first feed switch is used for direct feeding; The second feed switch is connected to a slurry mixer, which is used to stir and mix different materials for output.

8. The liquid phase laser ablation macro-quantization production apparatus according to claim 1, characterized in that, A discharge pump is connected between the input end of the catalyst slurry temporary storage device and the output end of the reaction chamber.

9. The liquid phase laser ablation macro-quantization production apparatus according to claim 1, characterized in that, The monitoring device includes thermocouples and temperature monitors; The thermocouple is disposed on the reaction chamber and is used to detect the internal temperature of the reaction chamber; The temperature monitor is configured to send the detection result of the thermocouple to the controller.

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