Gradient regulation type nano active silicon particle size synthesis reaction device

Abstract

The utility model discloses a gradient regulation type nanometer active silicon particle size synthesis reaction device, which relates to the technical field of nanometer active silicon particle size synthesis reaction devices and comprises an active silicon reaction kettle, a cavity is arranged in the active silicon reaction kettle, and an electric heating plate is sleeved in the cavity. The inner wall of the active silicon reaction kettle is fixedly connected with an ultrasonic assembly. According to the gradient regulation and control type nano active silicon particle size synthesis reaction device, through cooperative coupling of the electric heating plate and the ultrasonic assembly, the ultrasonic generator drives the multiple ultrasonic transducers which are symmetrically distributed to form a uniform cavitation field, and meanwhile the electric heating plate dynamically adjusts a temperature field based on a control panel instruction; space-time matching optimization of a temperature-cavitation dual-energy field is achieved, reaction nonuniformity caused by energy field separation of traditional equipment is effectively overcome, ultrasonic hot spots in the reaction kettle are eliminated through ultrasonic transducers which are arranged on a connecting rod in an axial symmetry mode, nano silicon particle nucleation growth kinetics are controllable, and the particle size standard deviation is reduced.

Description

Technical Field

[0001] This utility model relates to the technical field of nano-active silicon particle size synthesis reaction device, specifically a gradient-controlled nano-active silicon particle size synthesis reaction device. Background Technology

[0002] Traditional nano-silicon material synthesis processes generally suffer from problems such as single reaction conditions and wide particle size distribution. Existing reaction devices mostly use fixed parameter heating or mechanical stirring methods, lacking real-time particle size monitoring and dynamic control mechanisms, making it difficult to achieve gradient particle size control.

[0003] However, current nano-active silicon synthesis devices generally employ a single heat source or independent ultrasonic equipment. The temperature control of the heating plate and the ultrasonic energy field are often controlled separately, resulting in poor synergy between temperature and cavitation effects and an inability to achieve optimal energy field coupling. Existing technologies often rely on manual parameter switching in stages for gradient control, lacking a dynamic feedback mechanism based on real-time particle size data. This leads to a lag in the coordination between the temperature field and the ultrasonic field, significant fluctuations in the standard deviation of particle size distribution, and difficulty in adapting to the continuous gradient adjustment requirements of complex synthesis pathways.

[0004] Therefore, this invention provides a gradient-controlled nano-active silicon particle size synthesis reaction device. Utility Model Content

[0005] To address the shortcomings of existing technologies, this invention provides a gradient-controlled nano-active silicon particle size synthesis reaction device, which solves the problems of poor temperature-cavitation effect synergy caused by the separation of temperature control by the electric heating plate and the ultrasonic energy field; and the lack of a dynamic feedback mechanism based on real-time particle size data, resulting in a lag in the synergy between the temperature field and the ultrasonic field.

[0006] To achieve the above objectives, this utility model is implemented through the following technical solution: a gradient-controlled nano-active silicon particle size synthesis reaction device, including an active silicon reactor, wherein an active silicon reactor has an internal cavity and an electric heating plate is sleeved inside the cavity, an ultrasonic component is fixedly connected to the inner wall of the active silicon reactor, a dynamic control component is provided on the surface of the ultrasonic component, and an observation port is provided on the side of the active silicon reactor and an observation plate is sleeved inside the observation port;

[0007] The ultrasonic component includes a bracket fixedly connected to the inner wall of the activated silicon reactor. An equipment box is fixedly connected to the top surface of the bracket, and an ultrasonic generator is sleeved inside the equipment box. A connecting rod is fixedly connected to the bottom surface of the bracket on an axisymmetric basis, and multiple ultrasonic transducers are fixedly connected to the surface of the connecting rod.

[0008] The dynamic control component includes a control board fixedly connected to the top surface of the support and a dynamic light scattering detection module fixedly connected to the bottom surface of the support.

[0009] Preferably, the ultrasonic transducers are axially symmetrically and uniformly distributed along the length of the connecting rod.

[0010] Preferably, the dynamic light scattering detection module is located at the center of the bottom surface of the bracket and is electrically connected to the control board.

[0011] Preferably, the control board is electrically connected to the heating plate and the ultrasonic generator via wires.

[0012] Preferably, there are two connecting rods, and each connecting rod has multiple ultrasonic transducers fixedly connected to its surface.

[0013] Preferably, the observation plate is made of high-temperature resistant tempered glass and has a transparent protective layer on its outer surface.

[0014] Beneficial effects

[0015] This invention provides a gradient-controlled nano-sized active silicon particle synthesis reaction device. Compared with the prior art, it has the following advantages:

[0016] 1. This gradient-controlled nano-active silicon particle size synthesis reaction device, through the synergistic coupling of the heating plate and the ultrasonic component, the ultrasonic generator drives multiple axisymmetrically distributed ultrasonic transducers to form a uniform cavitation field. At the same time, the heating plate dynamically adjusts the temperature field based on the control board command, realizing the spatiotemporal matching optimization of the temperature-cavitation dual energy fields. This effectively overcomes the reaction non-uniformity caused by the energy field separation of traditional equipment. The ultrasonic transducers arranged axisymmetrically on the connecting rod eliminate ultrasonic hot spots in the reactor, making the nucleation and growth kinetics of nano-silicon particles controllable and reducing the standard deviation of particle size.

[0017] 2. This gradient-controlled nano-active silicon particle size synthesis reaction device monitors particle size distribution data in real time through a dynamic light scattering detection module and feeds it back to the control board. The heating power of the heating plate and the output frequency of the ultrasonic generator are adjusted synchronously through wires to form a closed-loop gradient control system. This solves the lag problem of traditional manual staged control, shortens the dynamic control response time, and realizes continuous synchronous gradual change of temperature field and ultrasonic field parameters, meeting the precise control requirements of particle size range in complex gradient synthesis processes. Attached Figure Description

[0018] Figure 1 This is a three-dimensional schematic diagram of the overall appearance of this utility model;

[0019] Figure 2 This is a three-dimensional schematic diagram of the electric heating plate of this utility model;

[0020] Figure 3 This is a three-dimensional appearance diagram of the ultrasonic component and the dynamic control component of this utility model;

[0021] Figure 4This is a cross-sectional three-dimensional appearance diagram of the present utility model.

[0022] In the diagram: 1. Activated silicon reactor; 2. Heating plate; 3. Ultrasonic assembly; 31. Support; 32. Equipment box; 33. Ultrasonic generator; 34. Connecting rod; 35. Ultrasonic transducer; 4. Dynamic control assembly; 41. Control board; 42. Dynamic light scattering detection module; 5. Observation board. Detailed Implementation

[0023] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.

[0024] This utility model provides two technical solutions:

[0025] Figures 1-4 The first embodiment is shown: a gradient-controlled nano-active silicon particle size synthesis reaction device, including an active silicon reactor 1, an internal cavity of the active silicon reactor 1 and a heating plate 2 sleeved in the cavity, an ultrasonic component 3 fixedly connected to the inner wall of the active silicon reactor 1, a dynamic control component 4 provided on the surface of the ultrasonic component 3, an observation port opened on the side of the active silicon reactor 1 and an observation plate 5 sleeved inside the observation port; the ultrasonic component 3 includes a bracket 31 fixedly connected to the inner wall of the active silicon reactor 1, an equipment box 32 fixedly connected to the top surface of the bracket 31 and an ultrasonic generator 33 sleeved inside the equipment box 32, a connecting rod 34 fixedly fixedly connected to the bottom surface of the bracket 31 on an axisymmetric basis, and a plurality of ultrasonic transducers 35 fixedly connected to the surface of the connecting rod 34.

[0026] Specifically, the heating plate 2 is embedded in the bottom of the cavity of the active silicon reactor 1 and receives the PWM voltage regulation signal from the control board 41 through wires. It heats the reaction system according to a preset gradient curve within the range of 50-200℃. In the ultrasonic component 3, the ultrasonic generator 33 in the equipment box 32 outputs a high-frequency electrical signal of 20-100kHz, which drives multiple ultrasonic transducers 35 symmetrically distributed on the two connecting rods 34 to synchronously excite cavitation bubbles. The distance between adjacent transducers is 1 / 6 of the reactor diameter to ensure that the cavitation field forms a uniform energy gradient in the radial direction. At the same time, the control board 41 dynamically adjusts the heating power of the heating plate 2 according to the temperature feedback, so that the temperature field and the cavitation field intensity are matched in a 1:1.2 ratio in three-dimensional space to achieve the directional nucleation of nano-silicon particles.

[0027] In this embodiment, the dynamic control component 4 includes a control board 41 fixedly connected to the top surface of the bracket 31 and a dynamic light scattering detection module 42 fixedly connected to the bottom surface of the bracket 31.

[0028] Specifically, the dynamic light scattering detection module 42 captures particle size distribution data at a sampling frequency of 10Hz at the center of the bottom surface of the support 31, and transmits the D50 value to the control board 41 in real time via RS485 bus. When the detected particle size deviation exceeds ±3nm, the control board 41 synchronously generates the heating rate command of the heating plate 2 and the frequency switching curve of the ultrasonic generator 33. The heating slope of the heating plate increases by 5℃ / min, which corresponds to an increase of 8kHz in the ultrasonic frequency. The two are coupled and controlled by the PID algorithm, and the parameter adjustment is completed within 0.3 seconds, so that the particle size growth rate is stabilized at 0.8nm / min. Finally, the continuous synthesis of three-stage gradient particle size products of 50nm, 100nm and 150nm is achieved in a single reaction.

[0029] Figures 1-4 The second embodiment is shown, the main difference from the first embodiment is that the control board 41 is electrically connected to the heating plate 2 and the ultrasonic generator 33 respectively through wires;

[0030] Specifically, the control board 41 is connected to the temperature control interface of the heating plate 2 and the drive port of the ultrasonic generator 33 via multi-core shielded wires. The heating plate wires are made of PTFE insulated high-temperature resistant cable, which can withstand temperatures up to 250℃. The ultrasonic generator wires are made of coaxial cable to transmit high-frequency electrical signals. During implementation, the control board 41 has a built-in dual-channel PID controller to analyze the temperature feedback signal and the ultrasonic frequency command respectively. When the dynamic light scattering detection module 42 detects the particle size deviation, the control board 41 sends a 0-10V analog voltage regulation signal to the heating plate 2 through the wires, and at the same time outputs a PWM frequency modulation pulse to the ultrasonic generator 33 to achieve millisecond-level coordinated adjustment of heating power and ultrasonic energy. This connection method reduces the adjustment delay of temperature field and ultrasonic field parameters to less than 0.2 seconds, which improves the response speed by 3 times compared with the traditional split-line control mode, ensuring that the energy field parameters accurately match the preset gradient curve during particle size growth.

[0031] An observation port is provided on the side of the active silicon reactor 1, and an observation plate 5 is fitted inside the observation port. The observation plate 5 is made of high-temperature resistant tempered glass and has a transparent protective layer on its outer surface.

[0032] Specifically, the observation plate 5 is made of double-layer borosilicate tempered glass with a thickness of 8mm. It can withstand temperatures up to 300℃ and has a light transmittance of ≥92%. The outer surface is coated with a 50nm thick transparent silicon nitride protective layer by magnetron sputtering. During implementation, the observation plate 5 is embedded in the observation port on the side wall of the reactor 1 with high-temperature sealant. The protective layer makes the surface hardness reach level 9H, resisting micro-jet impact corrosion under ultrasonic cavitation and eliminating the fogging phenomenon on the glass surface. Operators can directly observe the turbulent morphology and bubble distribution density of the reaction liquid through the observation plate 5. The dynamic light scattering detection module 42 is used to verify the reaction process. Compared with the traditional quartz observation window, the maintenance frequency is reduced by 60%, and there is no light transmittance decay during continuous reaction.

[0033] Furthermore, any content not described in detail in this specification is existing technology known to those skilled in the art.

[0034] Working principle: When the activated silicon reactor 1 is started, the heating plate 2 heats the reaction system according to the preset gradient curve. At the same time, the ultrasonic generator 33 outputs high-frequency electrical signals to multiple axisymmetrically distributed ultrasonic transducers 35 on the connecting rod 34 to excite a uniform cavitation field. The dynamic light scattering detection module 42 collects the particle size distribution data in the reaction liquid in real time and transmits the data to the control board 41 on the top of the support 31. When the particle size deviation exceeds the set threshold, the control board 41 adjusts the PID temperature control parameters of the heating plate 2 and the output frequency of the ultrasonic generator 33 synchronously through the wires. The axisymmetrically arranged ultrasonic transducers 35 on the connecting rod 34 eliminate local energy eddies under the superposition of the cavitation field, so that a three-dimensional uniform sound pressure gradient field is formed in the reactor 1. Combined with the radial temperature gradient distribution of the heating plate 2, the continuous and controllable growth of nano-silicon particles is realized. The high-temperature resistant and light-transmitting structure of the observation plate 5 allows the operator to visually verify the consistency between the cavitation bubble distribution density and the data of the dynamic light scattering detection module 42, forming a gradient control system with closed-loop feedback of temperature, ultrasound and particle size.

[0035] It should be noted that, in this document, relational terms such as "first" and "second" are used only to distinguish one entity or operation from another, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Furthermore, the terms "comprising," "including," or any other variations thereof are intended to cover non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements includes not only those elements but also other elements not expressly listed, or elements inherent to such process, method, article, or apparatus.

[0036] Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the present invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A gradient control type nano-active silicon particle size synthesis reaction device, comprising an active silicon reaction kettle (1), characterized in that: The activated silicon reactor (1) has an internal cavity and an electric heating plate (2) is fitted inside the cavity. An ultrasonic component (3) is fixedly connected to the inner wall of the activated silicon reactor (1). A dynamic control component (4) is provided on the surface of the ultrasonic component (3). An observation port is provided on the side of the activated silicon reactor (1) and an observation plate (5) is fitted inside the observation port. The ultrasonic component (3) includes a bracket (31) fixedly connected to the inner wall of the activated silicon reactor (1). The top surface of the bracket (31) is fixedly connected to an equipment box (32), and an ultrasonic generator (33) is sleeved inside the equipment box (32). The bottom surface of the bracket (31) is axially symmetrically connected to a connecting rod (34), and a plurality of ultrasonic transducers (35) are fixedly connected to the surface of the connecting rod (34). The dynamic control component (4) includes a control board (41) fixedly connected to the top surface of the bracket (31) and a dynamic light scattering detection module (42) fixedly connected to the bottom surface of the bracket (31).

2. The gradient control nano-active silicon particle size synthesis reaction device according to claim 1, characterized in that: The ultrasonic transducers (35) are evenly distributed along the length of the connecting rod (34) in an axisymmetric manner.

3. The gradient control nano-active silicon particle size synthesis reaction device according to claim 1, characterized in that: The dynamic light scattering detection module (42) is located at the center of the bottom surface of the bracket (31) and is electrically connected to the control board (41).

4. The gradient control nano-active silicon particle size synthesis reaction device according to claim 1, characterized in that: The control board (41) is electrically connected to the heating plate (2) and the ultrasonic generator (33) via wires.

5. The gradient-controlled nano-active silicon particle size synthesis reaction device according to claim 1, characterized in that: The number of connecting rods (34) is two, and each connecting rod (34) has multiple ultrasonic transducers (35) fixedly connected to its surface.

6. The gradient-controlled nano-active silicon particle size synthesis reaction device according to claim 1, characterized in that: The observation plate (5) is made of high-temperature resistant tempered glass and has a transparent protective layer on its outer surface.

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