A device and method for programmable laser heating nanomaterials for rapid synthesis

Abstract

The present application relates to the technical field of synthetic equipment, in particular to a programmable laser heating nanomaterial rapid synthesis device and method. The device comprises a support platform, a moving mechanism, a laser assembly and a program control system. The support platform has a plurality of accommodation spaces for installing reaction containers. The moving mechanism is installed on the support platform. The laser assembly is connected with the moving mechanism and used for emitting laser. The moving mechanism drives the laser assembly to move in X-axis, Y-axis or / and Z-axis direction under the manual control or automatic control of the program control system, so that the laser assembly emits laser along the Z-axis direction to at least one preset reaction container below, thereby heating the reactants in the reaction container and making the nanomaterial in the reactants react. The present application has high reaction efficiency, wide reaction range and small error, and can manually or automatically control multiple reactions to be carried out simultaneously.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of synthesis equipment, in particular to a programmable laser heating nanomaterial rapid synthesis device and method. BACKGROUND

[0002] High-quality nanocrystals have shown strong application potential in the fields of energy, catalysis, photovoltaics and display. The material and its spatial arrangement determine the function of the nanocrystals, and their interface controls the electronic and magnetic coupling. Therefore, reasonable preparation of heterostructure nanocrystals, which connect semiconductors with appropriate band gap and band edge positions, can make directional transport of electrons and holes, and be used in photocatalytic water splitting, photon upconversion, light-responsive light-emitting diodes and photodetectors.

[0003] Cation exchange method is a powerful post-treatment method for nanocrystals, and has excellent performance in the synthesis of heterostructure nanocrystals. At present, researchers have synthesized nanocrystals with doping structure, alloy structure, segmented structure and core-shell structure by using cation exchange method. Moreover, nanocrystals with rich composition and structure have also been obtained by sequential cation exchange method. Based on the characteristics of simple operation, mild conditions and good universality, cation exchange method has been widely used in the synthesis of nanomaterials.

[0004] Cation exchange reaction usually uses water bath method and oil bath method to heat the reaction system. However, water bath method is affected by the boiling point of water, and boiling phenomenon will occur when the temperature is close to the boiling point of water. Compared with water, oil bath can be heated to 100-250℃ at a higher temperature, and oil is less volatile, but the medium needs to be replaced after a long time of use to maintain the heating efficiency. Moreover, both heating methods are from outside to inside, and the uniformity and efficiency of heating are poor. In summary, both heating methods are limited by the intermediate heat transfer medium. These shortcomings greatly limit their application in automated processing.

[0005] The rise of artificial intelligence (AI) technology brings new development opportunities to many fields. At present, the application of AI technology in the field of chemistry is constantly expanding, from experimental operation to parameter simulation optimization, AI technology is deeply changing the face of chemical research. The synthesis of nanocrystals is a reaction that controls morphology, structure and composition at the nanoscale, which requires fine control. However, in terms of mechanism research, the experimental conditions and influencing factors of many nanosynthesis technologies need to be explored, which requires the advantages of automatic production and data analysis modeling of AI technology. Looking forward to the future, the deep integration of existing nanosynthesis technology and AI chemistry will become a key issue to promote the development of this field. SUMMARY

[0006] The present application aims to overcome the above-mentioned defects of the prior art, and provides a device and method for programmable laser heating of reactants for rapid synthesis.

[0007] To solve the above technical problems, the device for programmable laser heating of reactants for rapid synthesis provided by the technical solution of the present application comprises a support platform, a moving mechanism, a laser assembly and a program control system, wherein,

[0008] The support platform has a plurality of accommodation spaces for mounting reaction containers;

[0009] The moving mechanism is mounted to the support platform;

[0010] The laser assembly is connected to the moving mechanism and is used for emitting laser; wherein,

[0011] The moving mechanism drives the laser assembly to move in the X-axis, Y-axis or / and Z-axis direction under the manual control or automatic control of the program control system, so that the laser assembly emits laser along the Z-axis direction to at least one preset reaction container below, thereby heating the reactants in the reaction container and making the nanomaterials in the reactants react.

[0012] As an improvement of the above-mentioned device, the support platform comprises a height adjusting mechanism, an inclination adjusting mechanism and a support platform body, wherein the height adjusting mechanism is used for adjusting the height of the support platform body; the inclination adjusting mechanism is used for adjusting the inclination of the support platform body to ensure that the support platform body is in a horizontal position.

[0013] As an improvement of the above-mentioned device, the reaction container is mounted to the accommodation space along the Z-axis, and the top end is transparent to light.

[0014] As an improvement of the above-mentioned device, the moving mechanism comprises a first Y-direction lead screw sliding table, a second Y-direction lead screw sliding table, an X-direction lead screw sliding table and a Z-direction lead screw sliding table, wherein the first Y-direction lead screw sliding table and the second Y-direction lead screw sliding table are arranged along the Y-axis direction, are respectively mounted to two side edges of the top surface of the support platform, and are used for driving the laser assembly to move in the Y-axis direction; the X-direction lead screw sliding table is arranged along the X-axis direction, is connected to the upper side of the first Y-direction lead screw sliding table and the second Y-direction lead screw sliding table, and is used for driving the laser assembly to move in the X-axis direction; and the Z-direction lead screw sliding table is arranged along the Z-axis direction, is mounted to the X-direction lead screw sliding table, and is used for driving the laser assembly to move in the Z-axis direction.

[0015] As an improvement of the above device, the laser assembly comprises a laser, a laser power supply, an optical fiber and an optical corrector, wherein the laser power supply is used to power the laser and control the wavelength and / or intensity of the laser emitted by the laser through adjusting the power supply; the laser is connected with one end of the optical fiber, and the other end of the optical fiber is connected with the optical corrector installed on the moving mechanism, so that the laser emitted by the laser is transmitted to the optical corrector and emitted to the reaction container below the optical corrector along the Z-axis direction after being corrected.

[0016] As an improvement of the above device, the optical corrector is installed on the moving mechanism through a clamp, and the clamp is provided with at least one installation position of the optical corrector.

[0017] As an improvement of the above device, the optical corrector comprises a collimator and a device for expanding the light spot.

[0018] As an improvement of the above device, the program control system comprises a driver, a control cabinet and an upper computer.

[0019] The control cabinet is provided with a manual control button; the upper computer comprises a programming control module and / or an AI control module; wherein the program control system has a manual adjustment mode, the driver is controlled through the manual button of the control cabinet, the moving mechanism is driven to move through the driver, so as to drive the laser assembly to move and emit the laser to the predetermined reaction container; the program control system also has an automatic adjustment mode, the driver is automatically controlled through the programming control module and / or the AI control module of the upper computer, the moving mechanism is driven to move through the driver, so as to drive the laser assembly to move and emit the laser to the predetermined reaction container.

[0020] As an improvement of the above device, a magnetic stirrer is further included, which is used to stir the reactant in the reaction container, and the reactant comprises a nano material.

[0021] In order to achieve another object of the present application, the present application further provides a rapid synthesis method of reactant, which is realized based on the above device for programmable laser heating of reactant rapid synthesis and comprises the following steps:

[0022] Adjust the support platform to a horizontal position;

[0023] Install the reaction container, fill the reactant and magnetic particles into the reaction container, and stir through the magnetic stirrer;

[0024] Start the laser assembly to preheat and stabilize the output laser;

[0025] The laser assembly is moved by the moving mechanism controlled by the program control system manually or automatically, so that the laser emits along the Z-axis direction to at least one preset reaction container below, so as to heat the reactants in the reaction container and make the reactants react.

[0026] Compared with the prior art, the present application has the following advantages:

[0027] 1. The present application uses the combined screw slide table to control the reaction fixed point and time, and is automatically performed. The movement and stop of the screw slide table are manually or automatically controlled by the control cabinet, and the movement distance, the residence time and the movement speed parameters have good flexibility and adjustability, which not only reduces the error caused by manual operation, but also avoids the harm to the operator caused by the laser during the operation.

[0028] 2. The present application uses the laser irradiation to make the nanocrystal generate heat and thus excite the cation exchange reaction, which is in-situ heat generation, effectively avoiding the limitation caused by the influence of the traditional heat transfer medium. At the same time, the in-situ heat generation efficiency is higher, which can greatly improve the reaction efficiency.

[0029] 3. The present application uses the laser irradiation reaction mode, and the reaction position is controlled by the laser irradiation position, so that the fixed point reaction can be accurately performed. However, by replacing other laser conversion devices, large-scale reaction can also be performed.

[0030] 4. The present application can use multiple groups of lasers or use conversion devices to expand the laser range to achieve simultaneous control of multiple reactions.

[0031] 5. The present application uses the control cabinet 6 to control the screw slide table, and performs the movement and stop operation. In addition to the control by the control cabinet 6, the program control or the connection with AI can also be performed. DETAILED DESCRIPTION

[0032] The accompanying drawings are included to provide a further understanding of the present application, and constitute a part of the specification, which together with the embodiments of the present application, are used to explain the present application, and do not constitute a limitation of the present application.

[0033] Figure 1 The structure schematic diagram of the programmable laser heating nanomaterial rapid synthesis device provided for the embodiments of the present application;

[0034] Figure 2 The partial enlarged view of the connection between the clamp and the end collimator;

[0035] Figure 3 The TEM image of the nanocrystal synthesized by the conventional water bath device;

[0036] Figure 4The image shows a TEM image of nanocrystals synthesized using the apparatus for rapid synthesis of reactants via programmable laser heating provided in this embodiment of the invention.

[0037] Attached Figure Labels

[0038] 1. First Y-direction lead screw slide table; 2. Second Y-direction lead screw slide table; 3. X-direction lead screw slide table.

[0039] 4. Z-direction lead screw slide table; 5. Stepper motor; 6. Control cabinet.

[0040] 7. Fixture; 8. End collimator; 9. Optical fiber

[0041] 10. Laser; 11. Laser power supply; 12. Support platform

[0042] 13. Reaction vessel 14. Magnetic stirrer Detailed Implementation

[0043] The present invention will be further described below with reference to the accompanying drawings and specific embodiments, but is not limited thereto. The described embodiments are only some embodiments of the present invention, and not all embodiments. 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.

[0044] Example 1

[0045] like Figure 1 As shown, this invention provides a programmable laser-heated rapid synthesis device for nanomaterials. The device includes a moving mechanism. This moving mechanism comprises a first Y-direction lead screw slide 1, a second Y-direction lead screw slide 2, an X-direction lead screw slide 3, and a Z-direction lead screw slide 4. The first Y-direction lead screw slide 1, the second Y-direction lead screw slide 2, and the X-direction lead screw slide 3 are interconnected in an H-shape. The first Y-direction lead screw slide 1 and the second Y-direction lead screw slide 2 control forward and backward movement along the Y-axis, while the X-direction lead screw slide 3 controls left and right movement along the X-axis. The Z-direction lead screw slide 4 is interconnected with the X-direction lead screw slide 3 and controls up and down movement along the Z-axis. The four lead screw slides are connected to four stepper motors 5 to control rotation. A control cabinet 6 manually / automatically controls the four stepper motors 5. Figure 2 As shown, a collimator 8 is connected to the Z-direction lead screw slide 4 using a clamp 7. The collimator 8 is connected to the laser 10 via an optical fiber 9, allowing the laser to be emitted in a straight line. The laser power supply 11 can supply power to the laser 10, switch the laser on and off, and adjust the output power. The entire device is placed on a support platform 12, which can be adjusted in height and tilt to ensure the entire device is placed horizontally. The support platform 12 also provides space for the reaction vessel 13 and the magnetic stirrer 14.

[0046] In this embodiment, controlled by the control cabinet 6, the moving mechanism, driven by the stepper motor 5, is responsible for driving the laser to move and stop at fixed points and times in the X, Y, and Z axes. The specific moving distance, speed, and dwell time are controlled by the control cabinet 6, thereby controlling the specific reaction position and reaction time. The control cabinet 6 can be set to manual mode, i.e., by pressing different buttons or inputting different parameters to control the stepper motor 5 to rotate forward or backward, thereby controlling the laser's movement up, down, left, right, forward, and backward; or it can be set to automatic mode, i.e., by setting a program, the stepper motor 5 will automatically rotate according to the program requirements, thereby controlling the laser to move in a certain way. The control cabinet 6 can be connected to a computer to control the operation of the stepper motor 5 through programming. The control cabinet 6 can also be combined with AI technology. Similarly, this control can also be directly controlled by programming or connected to AI for control.

[0047] In this embodiment, the fixture 7 is connected to the Z-direction lead screw slide 4, and the Z-direction lead screw slide 4 is also connected to the laser end collimator 8. Figure 1 An embodiment is shown with one end collimator 8 connected. However, in other embodiments, the clamp 7 can connect several end collimators 8, forming an array laser to achieve multi-site synthesis or combined screening. This embodiment utilizes the end collimator 8 to focus the laser, ensuring a straight laser beam. However, in other embodiments, it can be replaced with other end straighteners (such as devices for expanding the beam) or laser conversion devices located at the laser's end exit port, depending on the required response.

[0048] The reactants are placed in reaction vessel 13, and the reaction is completed by heating with laser irradiation. The reactor can be... Figure 1 The reaction vessel 13 shown is not applicable; however, other reaction vessels conforming to the operating principles of this device may also be used. Reaction vessel 13 may include conventional reaction vessels and sealed reaction vessels. The plane of the opening of a conventional reaction vessel should be perpendicular to the laser beam path; for a sealed reaction vessel, the light-transmitting surface should be perpendicular to the laser beam path. Other types of reaction vessels should adhere to the principle of light transmission and sufficient contact between the reaction system and the light. The laser heating mechanism includes spontaneous heat generation from the material due to the photothermal effect and / or the direct thermal effect of the laser on the material and solvent.

[0049] In this embodiment, laser 10 is used to emit laser light. The optical parameters such as the wavelength and power of the laser emitted by laser 10 can be adjusted according to the reaction conditions.

[0050] Example 2

[0051] This embodiment provides a method for rapid synthesis of nanomaterials, which is implemented based on a device for rapid synthesis of nanomaterials using programmable laser heating.

[0052] In the embodiment, the reaction substance is filled in the reaction container 13, and different reaction containers can be replaced according to the reaction requirement. During the reaction, the magnetic particles with proper size can be added, and the magnetic stirrer 14 is used to stir and mix uniformly. The end collimator 8 can be replaced by other conversion devices according to the requirement, so that the emitted light spot meets the reaction requirement. The power of the laser can be adjusted by the laser power supply 11, and different lasers 10 can be replaced to emit laser with different wavelengths.

[0053] Working principle: first, adjust the support platform 12 to the horizontal state, select the appropriate reaction container 13, fill the reaction substance and magnetic particles therein, place it on the magnetic stirrer 14, start the magnetic stirrer 14 and select the appropriate rotating speed for stirring. Turn on the laser power supply 11, adjust the laser power, then turn on the laser, the laser is emitted from the laser 10, passes through the optical fiber 9 and the end collimator 8, and is emitted, after preheating for about 5 minutes, the laser can be stably output. Determine the zero point by using the control cabinet 6 in manual mode, input the position parameter, time parameter and speed parameter in automatic mode, and start running. The stepping motor 5 drives the first Y direction lead screw sliding table 1, the second Y direction lead screw sliding table 2, the X direction lead screw sliding table 3 and the Z direction lead screw sliding table 4 to slide according to the input parameters, so that the laser can move to the required position and stay, under the irradiation of the laser, the reaction substance in the reaction container 13 reacts. After the reaction is completed, the reaction container 13 is taken out and the reaction substance is taken away. Turn off the laser, and take down the end collimator 8 from the clamp 7 for cleaning.

[0054] The device and method for programmable laser heating of nanomaterial reaction substance rapid synthesis provided by the application can be used for the reaction of cation exchange:

[0055]

[0056] Figure 3 The TEM image of nanocrystals synthesized by the traditional water bath device is shown; Figure 4 The TEM image of nanocrystals synthesized by the device for programmable laser heating of nanomaterial rapid synthesis provided by the embodiment of the application is shown.

[0057] Finally, it should be noted that: the above only describes the preferred embodiments of the application, and is not used to limit the application, although the application has been described in detail with reference to the foregoing embodiments, for those skilled in the art, the technical solutions recorded in the foregoing embodiments can be modified, or some technical features can be replaced. Any modification, equivalent replacement, improvement, etc. made within the spirit and principles of the application shall be included in the protection scope of the application.

Claims

1. A method for rapidly synthesizing nanomaterials, based on a device for rapidly synthesizing nanomaterials by programmable laser heating; The apparatus comprises: a support platform, a moving mechanism, a laser assembly, and a program control system, wherein the support platform has a plurality of accommodation spaces for mounting reaction vessels; the moving mechanism is mounted to the support platform; the laser assembly is connected to the moving mechanism and is used for emitting laser light; wherein the moving mechanism drives the laser assembly to move in the X-axis, Y-axis, or / and Z-axis direction under the manual or automatic control of the program control system, so that the laser assembly emits laser light along the Z-axis direction into at least one predetermined reaction vessel below, thereby heating the reactants in the reaction vessel and making the nanomaterials in the reactants react; the support platform comprises a height adjusting mechanism, an inclination adjusting mechanism, and a support platform body, wherein the height adjusting mechanism is used to adjust the height of the support platform body; the inclination adjusting mechanism is used to adjust the inclination of the support platform body to ensure that the support platform body is in a horizontal position; the reaction vessel is mounted to the accommodation space along the Z-axis, and the top end is transparent to light; the moving mechanism comprises a first Y-direction lead screw sliding table, a second Y-direction lead screw sliding table, an X-direction lead screw sliding table, and a Z-direction lead screw sliding table, wherein the first Y-direction lead screw sliding table and the second Y-direction lead screw sliding table are arranged along the Y-axis direction and are respectively mounted to the two side edges of the top surface of the support platform, and are used to drive the laser assembly to move in the Y-axis direction; the X-direction lead screw sliding table is arranged along the X-axis direction and is connected above the first Y-direction lead screw sliding table and the second Y-direction lead screw sliding table, and is used to drive the laser assembly to move in the X-axis direction; the Z-direction lead screw sliding table is arranged along the Z-axis direction and is mounted to the X-direction lead screw sliding table, and is used to drive the laser assembly to move in the Z-axis direction; the laser assembly comprises a laser, a laser power supply, an optical fiber, and an optical corrector, wherein the laser power supply is used to power the laser and control the wavelength and / or intensity of the laser light emitted by the laser by adjusting the power supply; the laser is connected to one end of the optical fiber, and the other end of the optical fiber is connected to the optical corrector mounted to the moving mechanism, so that the laser light emitted by the laser is transmitted to the optical corrector and emitted along the Z-axis direction into the reaction vessel below after correction; the program control system comprises a driver, a control cabinet, and an upper computer; the control cabinet is provided with a manual control button; the upper computer comprises a programming control module and / or an AI control module; wherein the program control system has a manual adjustment mode, the driver is controlled by the manual button of the control cabinet, and the moving mechanism is driven by the driver to move, thereby driving the laser assembly to move and emitting laser light into the predetermined reaction vessel; the program control system also has an automatic adjustment mode, the driver is automatically controlled by the programming control module and / or the AI control module of the upper computer, and the moving mechanism is driven by the driver to move, thereby driving the laser assembly to move and emitting laser light into the predetermined reaction vessel; the device further comprises a magnetic stirrer, which is used to stir the reactants in the reaction vessel. The method comprises the following steps: adjusting the support platform to a horizontal position; installing the reaction container, filling the reaction material and magnetic particles into the reaction container, and stirring by the magnetic stirrer; starting the laser assembly to preheat and stabilize the output laser; controlling the movement mechanism to move the laser assembly by the program control system manually or automatically, so that the laser emits along the Z-axis direction to at least one preset reaction container below, to heat the reaction material in the reaction container and make the reaction material react.

2. The method of claim 1, wherein the nanoparticles are synthesized in less than 30 minutes. The optical corrector is installed to the movement mechanism by a clamp, and the clamp is provided with at least one installation position of the optical corrector.

3. The method of claim 1, wherein the nanomaterial is synthesized in less than 10 minutes. The optical corrector comprises a collimator and a device for expanding or reducing the light spot.

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