Precursor rectification device, system and method for semiconductor

Abstract

The invention discloses a semiconductor precursor rectification device, system and method, the semiconductor precursor rectification device comprises a heat exchange assembly, a distribution assembly and a liquid collection assembly, the distribution assembly comprises a distribution pipe body, and the bottom of the distribution pipe body is provided with a connecting hole for a rectification tower to convey steam; the liquid collection assembly is arranged between the distribution pipe body and the heat exchange assembly and comprises an extractor used for collecting liquid generated by condensation of the heat exchange assembly, a base plate is arranged at the bottom of the extractor, an overflow pipe and a plurality of gas-phase circulation pipes are arranged on the base plate, and the gas-phase circulation pipes are communicated with the extractor and the distribution pipe body; one end of the overflow pipe extends into the extractor to form an overflow port, and the other end of the overflow pipe extends into the distribution assembly and is positioned above the connecting hole, so that condensed liquid can be in contact with steam discharged from the rectifying tower in the distribution pipe body, heavy component substances in the steam are flushed, and then the heavy component substances flow back into the rectifying tower together; corresponding light component substances can be quickly enriched and discharged in time, so that the content of the light component substances in the semiconductor precursor is reduced.

Description

Technical Field

[0001] The present invention relates to the technical field of semiconductor materials, and particularly to a rectification device, system and method for semiconductor precursors. Background Art

[0002] As semiconductor manufacturing processes advance towards 5-nanometer and below technology nodes, the preparation of high-purity semiconductor precursors (such as metal organic compounds, halides, etc.) has become a key challenge. The purity of semiconductor precursors directly affects chip performance and reliability. In particular, the residues of metal impurities, oxygen-containing pollutants, and particulate matter need to be controlled at the ppb (parts per billion) level, which poses almost extreme requirements on traditional chemical rectification technologies. However, there are significant differences between the purification scenarios of semiconductor precursors and the traditional chemical industry: the former needs to achieve impurity separation under small-batch and high-precision conditions, while the latter usually focuses on large-scale continuous production. Traditional chemical rectification usually processes ton-level materials and allows relatively large component fluctuations, while precursor rectification needs to achieve ppb-level impurity control with kilogram-level operation amounts. It is difficult to be compatible in terms of process design logic between the two.

[0003] Patent CN201384866Y provides a vertical automatic reflux and withdrawal rectification device. The device consists of a mist eliminator, a shell-and-tube condenser, a reflux and withdrawal controller, a top product outlet, a rectification column, a withdrawal flowmeter, a withdrawal regulating valve, and a reboiler at the bottom of the column. The material is evaporated by the reboiler at the bottom of the column, and after heat transfer and mass transfer inside the column, the material vapor enters the shell-and-tube condenser at the top of the column for condensation and then descends into the liquid collection tank of the reflux and withdrawal controller; the condensed liquid enters the annular liquid collection cavity from both ends of the liquid collection tank, and part of it is redirected and redistributed for reflux through the overflow holes on the side of the overflow weir by the guide cylinder, part of it is distributed through weep holes, and part of it is taken out as the finished product through the flowmeter and regulating valve at the top product outlet; the non-condensable gas is removed of liquid droplets through the mist eliminator and then drawn away from the top vacuum port.

[0004] However, although the vertical automatic reflux and withdrawal rectification device provided in the above patent is widely used in the traditional chemical industry, it exposes a series of limitations in the purification of semiconductor precursors. First of all, the number of theoretical plates and separation efficiency of the traditional device are difficult to meet the separation requirements of light and heavy components with similar boiling points, resulting in impurity residue levels far higher than the requirements of semiconductor processes, and it is also difficult to improve the separation efficiency. Summary of the Invention

[0005] Based on this, in view of the above problem of insufficient gas-liquid separation degree, it is necessary to provide a rectification device, system and method for semiconductor precursors.

[0006] The present application provides a rectification device for semiconductor precursors, including a heat exchange component, and further including: A distribution component, the distribution component includes a distribution pipe body, and a connection hole for delivering steam from a rectification column is provided at the bottom of the distribution pipe body; A liquid collection component disposed between the distribution pipe body and the heat exchange component, the liquid collection component includes a sampler for collecting the liquid condensed by the heat exchange component, a substrate is provided at the bottom of the sampler, an overflow pipe and a plurality of gas-phase flow pipes are arranged on the substrate, and the gas-phase flow pipes communicate the sampler with the distribution pipe body; one end of the overflow pipe extends into the sampler to form a liquid collection space with the side wall surface of the sampler, an overflow port is provided at the end of the overflow pipe extending into the sampler, and the other end extends into the distribution component and is located above the connection hole, so that the condensed liquid can contact the steam coming out of the rectification column in the distribution pipe body to wash the heavy component substances in the steam.

[0007] Optionally, the overflow pipe is located at the central position of the substrate, and a plurality of the gas-phase flow pipes are arranged around the overflow pipe.

[0008] Optionally, the height of the overflow port exceeds the substrate, so that when a certain amount of liquid accumulates in the sampler, it enters the overflow pipe through the overflow port.

[0009] Optionally, the overflow pipe and the connection hole are coaxially arranged, the inner diameter of the overflow pipe is not less than the diameter of the connection hole, and the liquid in the overflow pipe flows back into the rectification column through the connection hole.

[0010] Optionally, a first flange for connecting the rectification column is provided at the bottom of the distribution pipe body, and the connection hole is arranged on the first flange.

[0011] Optionally, an air outlet hole is opened at one end of the gas-phase flow pipe extending into the sampler, an air inlet hole is provided at the other end of the gas-phase flow pipe, and the air inlet hole is flush with the bottom surface of the substrate.

[0012] Optionally, the distance from the overflow port to the substrate is less than the distance from the air outlet hole to the substrate.

[0013] Optionally, the substrate and the side wall surface of the sampler are integrally formed.

[0014] Optionally, a second flange is provided on the outer side wall surface at the bottom of the liquid collection component, the second flange protrudes from the outer side wall surface of the liquid collection component, a third flange is provided on the outer side wall surface at the top of the distribution component, the third flange protrudes from the outer side wall surface of the distribution component, and the second flange and the third flange have the same diameter and are connected in cooperation to connect the liquid collection component and the distribution component.

[0015] Optionally, it further includes a first temperature control component. The first temperature control component includes a heating pipeline disposed inside the side wall of the extractor. The heating pipeline is wound inside the side wall of the extractor. The top of the heating pipeline is flush with the top of the overflow pipe and is connected to a heat source device for heating the liquid inside the extractor. The first temperature control component further includes a first temperature sensor for collecting the temperature of the liquid inside the extractor.

[0016] Optionally, it further includes a second temperature control component. The second temperature control component is connected to the overflow pipe for heating the liquid inside the overflow pipe.

[0017] Optionally, the air outlet is disposed on the side wall surface of the overflow pipe away from the substrate, and the top end surface of the gas-phase flow pipe away from the substrate is closed.

[0018] Optionally, the liquid collection component is provided with an extraction port. The extraction port is disposed on the side wall surface of the extractor close to the substrate. The distance from the extraction port to the substrate is less than the distance from the overflow port to the substrate. A concentration sensor is provided on the extraction port.

[0019] This application also provides a precursor rectification system for semiconductors, including the above-mentioned precursor rectification device for semiconductors, and further includes a rectification tower. The rectification tower is connected to the distribution component.

[0020] This application also provides a precursor rectification method for semiconductors. Using the above-mentioned precursor rectification system for semiconductors, it includes the following steps: Adjust the temperature of the rectification tower to the evaporation temperature T1, where T1 is between the boiling point Ta of the heavy component A and the boiling point Tb of the light component B in the liquid precursor inside the rectification tower.

[0021] Adjust the heat exchange component to the condensation temperature T2, where T2 is less than Tb. Collect the liquid condensed by the heat exchange component until the liquid accumulates in the extraction chamber and flows into the overflow pipe.

[0022] Adjust the first temperature control component until the temperature of the liquid in the extraction chamber reaches T3, where T3 is Tb * floating coefficient K1.

[0023] Adjust the second temperature control component until the temperature of the liquid in the overflow pipe reaches T4, where T4 is Tb * floating coefficient K2.

[0024] Continue evaporation until the concentration of the light component B in the liquid in the extraction chamber reaches the threshold, and determine that the liquid precursor in the rectification tower has completed light component removal.

[0025] Adopting the technical solution provided by this application, compared with the prior art, it has the following beneficial effects: The connection holes at the bottom of the distribution pipe body are connected to the steam outlet of the rectification column, enabling the rising steam to diffuse along the internal space of the distribution pipe body. The extractor of the liquid collection assembly forms an air path connection with the distribution pipe body through the gas-phase flow pipe on the substrate. The steam vertically enters the top space of the extractor through the gas-phase flow pipe and is further transported to the heat exchange assembly for condensation. During this process, the condensed liquid collected in the extractor flows reversely through the overflow pipe below the substrate. One end of the overflow pipe extends into the distribution pipe body and its overflow port is higher than the position of the connection hole, such that when the reflux liquid flows downward in the distribution pipe body, it forms a countercurrent contact with the newly rising steam entering from the connection hole. The condensed liquid scours the unvaporized heavy component liquid droplets or high-boiling substances entrained in the steam, forcing the heavy components to return to the rectification column with the liquid to participate in rectification again, while the light components in the steam enter the heat exchange assembly through the gas-phase flow pipe due to the boiling point difference. The uniform arrangement of the gas-phase flow pipes on the substrate not only ensures the uniform distribution of the steam flow rate, but also, through the physical barrier of the substrate to the liquid in the extractor, prevents the liquid from flowing back into the distribution pipe body when the steam pressure fluctuates. At the same time, the height of the overflow port limits the upper limit of the liquid level in the extractor. When the volume of the condensed liquid exceeds the height of the overflow port, the excess liquid automatically drains through the overflow pipe, which not only maintains the dynamic update of the light component condensed liquid in the extractor, but also prevents the liquid level from being too high and blocking the gas-phase flow pipe. The continuous condensation of the light component steam by the heat exchange assembly and the collection and discharge of the extractor form a closed loop, enabling the light component substances to be continuously concentrated and discharged from the system, while the heavy components are intercepted through the gas-liquid countercurrent contact and returned to the rectification column, reducing the enrichment of the heavy components at the top of the rectification column, and ultimately achieving the efficient removal of the light component impurities and the cyclic purification of the heavy components in the semiconductor precursor, improving the separation efficiency. Description of the Drawings

[0026] Figure 1 It is a cross-sectional structure diagram of a semiconductor precursor rectification device provided by an embodiment of the present application; Figure 2 It is a cross-sectional structure diagram of the liquid collection assembly and the distribution assembly of a semiconductor precursor rectification device provided by an embodiment of the present application; Figure 3 It is a structure diagram of the liquid collection assembly of a semiconductor precursor rectification device provided by an embodiment of the present application; Figure 4 It is a schematic diagram of the first temperature adjustment assembly of a semiconductor precursor rectification device provided by an embodiment of the present application; Figure 5 It is an external structure diagram of a semiconductor precursor rectification device provided by an embodiment of the present application.

[0027] Description of the Reference Numerals: 100, Heat exchange component; 200, Distribution component; 210, Distribution pipe body; 220, Connection hole; 230, First flange; 240, Third flange; 300, Liquid collection component; 310, Extractor; 320, Substrate; 330, Overflow pipe; 331, Overflow port; 340, Gas-phase flow pipe; 341, Air outlet hole; 342, Air inlet hole; 350, Second flange; 360, Extraction port; 370, Concentration sensor; 380, Liquid collection space; 400, First temperature regulation component; 410, Heating pipeline. Detailed implementation manners

[0028] To make the above objects, features, and advantages of the present invention more obvious and understandable, the following will describe the detailed implementation manners of the present invention with reference to the accompanying drawings. Many specific details are set forth in the following description to fully understand the present invention. However, the present invention can be implemented in many other ways different from those described herein. Those skilled in the art can make similar improvements without departing from the connotation of the present invention. Therefore, the present invention is not limited by the specific embodiments disclosed below.

[0029] In the description of the present invention, it should be understood that the terms "center", "longitudinal", "transverse", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc. indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. It is only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation. Therefore, it should not be construed as a limitation of the present invention.

[0030] In addition, the terms "first" and "second" are only used for descriptive purposes and cannot be understood as indicating or implying relative importance or implicitly specifying the quantity of the indicated technical features. Thus, the features defined with "first" and "second" may explicitly or implicitly include at least one of such features. In the description of the present invention, "a plurality" means at least two, such as two, three, etc., unless otherwise specifically and clearly defined.

[0031] In the present invention, unless otherwise clearly specified and limited, the terms "installed", "connected", "connected to", "fixed", etc. should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or integrated; it can be a mechanical connection or an electrical connection; it can be directly connected or indirectly connected through an intermediate medium. It can be the internal communication of two elements or the interaction relationship between two elements, unless otherwise clearly limited. For those of ordinary skill in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0032] Refer to Figures 1 to 3 , an embodiment of the present invention provides a semiconductor precursor rectification device, including a heat exchange component 100, and further including: A distribution component 200, the distribution component 200 includes a distribution pipe body 210, and a connection hole 220 for delivering steam to the rectification column is provided at the bottom of the distribution pipe body 210; A liquid collection component 300 disposed between the distribution pipe body 210 and the heat exchange component 100, the liquid collection component 300 includes a sampler 310 for collecting the liquid condensed by the heat exchange component 100, a substrate 320 is provided at the bottom of the sampler 310, an overflow pipe 330 and a plurality of gas-phase flow pipes 340 are arranged on the substrate 320, and the gas-phase flow pipes 340 communicate the sampler 310 with the distribution pipe body 210; one end of the overflow pipe 330 extends into the sampler 310 to form a liquid collection space 380 with the side wall surface of the sampler 310, an overflow port 331 is provided at the end of the overflow pipe 330 extending into the sampler 310, and the other end extends into the distribution component 200 and is located above the connection hole 220, so that the condensed liquid can contact the steam coming out of the rectification column in the distribution pipe body 210, realizing flushing of the heavy component substances in the steam, and then flowing back to the rectification column together. The corresponding light component substances can be rapidly enriched, and the light component substances are discharged in time, so that the content of the light component substances in the semiconductor precursor is reduced.

[0033] Refer to Figure 2 , in the figure, the downward arrow is the liquid condensed, the upward arrow is the steam generated by the rectification column, and the dotted box area is the area where the condensed liquid contacts the steam and produces a flushing effect.

[0034] In this embodiment, the connection hole 220 at the bottom of the distribution pipe body 210 is communicated with the steam outlet of the rectification column, so that the rising steam diffuses along the internal space of the distribution pipe body 210. The extractor 310 of the liquid collection assembly 300 forms an air path connection with the distribution pipe body 210 through the gas-phase flow pipe 340 on the substrate 320. The steam vertically enters the top space of the extractor 310 through the gas-phase flow pipe 340 and is further transported to the heat exchange assembly 100 for condensation. During this process, the condensed liquid collected in the extractor 310 flows reversely through the overflow pipe 330 below the substrate 320. One end of the overflow pipe 330 extends into the distribution pipe body 210 and its overflow port 331 is higher than the position of the connection hole 220, so that when the reflux liquid flows from top to bottom in the distribution pipe body 210, it forms a countercurrent contact with the newly rising steam entering from the connection hole 220. The condensed liquid scours the unvaporized heavy component droplets or high-boiling substances entrained in the steam, forcing the heavy components to return to the rectification column with the liquid to participate in rectification again, while the light components in the steam enter the heat exchange assembly 100 through the gas-phase flow pipe 340 due to the boiling point difference. The uniform arrangement of the gas-phase flow pipes 340 on the substrate 320 not only ensures the uniform distribution of the steam flow rate, but also avoids the backflow of the liquid into the distribution pipe body 210 when the steam pressure fluctuates through the physical barrier of the substrate 320 to the liquid in the extractor 310. At the same time, the height of the overflow port 331 limits the upper limit of the liquid level in the extractor 310. When the volume of the condensed liquid exceeds the height of the overflow port 331, the excess liquid automatically drains through the overflow pipe 330, which not only maintains the dynamic update of the light component condensed liquid in the extractor 310, but also avoids the liquid blocking the gas-phase flow pipe 340 due to too high a liquid level. The continuous condensation of the light component steam by the heat exchange assembly 100 and the collection and discharge of the extractor 310 form a closed loop, so that the light component substances are continuously concentrated and discharged from the system, while the heavy components are intercepted by the gas-liquid countercurrent contact and returned to the rectification column, reducing the enrichment of the heavy components at the top of the rectification column, and finally realizing the efficient removal of the light component impurities in the semiconductor precursor and the cyclic purification of the heavy components, improving the separation efficiency.

[0035] In the prior art, the condensed liquid generated by the shell-and-tube condenser needs to be refluxed and extracted through a multi-stage distribution structure such as a draft tube, an overflow weir and weep holes, and its separation efficiency is limited by the static overflow and passive diversion mechanism. For example, the overflow holes on the side of the overflow weir can only control the reflux amount through a fixed aperture, and although the capillary action of the weep holes can assist in liquid distribution, it is difficult to accurately adjust the extraction ratio of the light components. Especially when dealing with light and heavy component systems with close boiling points and subtle physical property differences, it is easy to cause secondary entrainment of the condensed liquid or residual light components. In addition, although the mist eliminator can intercept the liquid droplets in the gas phase, it cannot actively intercept the uncondensed heavy component molecules in the steam, and finally the light component content is difficult to break through the threshold of 2%.

[0036] Furthermore, the collaborative design of the gas-phase flow pipe 340 and the substrate 320 remedies the defect of the cross-interference of the gas-liquid path in the traditional device. The uniform arrangement of the gas-phase flow pipes 340 on the substrate 320 not only realizes the homogenized distribution of the steam flow rate, but also completely isolates the rising steam from the descending liquid through the physical barrier of the substrate 320, fundamentally eliminating the decrease in mass transfer efficiency caused by the mixing of gas-liquid two-phase flow in the prior art. For example, although the structure of the draft tube and the weep holes in the patent CN201384866Y can guide the liquid distribution, it cannot avoid the local mixing of the rising steam and the reflux liquid in the liquid collection tank, resulting in some light components being carried back into the tower by the reflux liquid. In this embodiment, through the spatial isolation of the substrate 320 and the directional diversion of the gas-phase flow pipe 340, it is ensured that the light-component steam reaches the condensation region directly under the condition of no interference, realizing the rapid enrichment and directional discharge of the light components.

[0037] Refer to Figures 1 to 3 , in one embodiment, the overflow pipe 330 is located at the central position of the substrate 320, and a plurality of gas-phase flow pipes 340 are arranged around the overflow pipe 330.

[0038] In this embodiment, the overflow pipe 330 is located at the central position of the substrate 320, and a plurality of gas-phase flow pipes 340 are arranged around the overflow pipe 330. This structural arrangement further optimizes the contact path and contact efficiency of the liquid and gas in the distribution pipe body 210. Specifically, the overflow pipe 330 at the central position enables the condensed liquid collected in the extractor 310 to preferentially flow back into the distribution pipe body 210 from the central region. At the same time, the structure surrounded by the gas-phase flow pipes 340 arranged around it makes the steam from the distribution pipe body 210 rise uniformly from the periphery to the substrate 320 and enter the extractor 310 through the gas-phase flow pipes 340 during the process of flowing towards the extractor 310.

[0039] This arrangement distributed from the center to the outside enables the gas phase and the liquid phase to achieve more sufficient and uniform contact in the distribution pipe body 210, enhancing the scouring effect of the condensed liquid on the heavy-component substances in the steam. At the same time, this layout helps to maintain the stability of the gas-liquid flow inside the device, avoiding local turbulence or uneven flow, thereby further improving the efficiency of the rectification process. Thus, this structure can more effectively realize the recovery of heavy components and the enrichment of light components, contributing to reducing the content of light-component substances in the final product and improving the purity of the semiconductor precursor.

[0040] Refer to Figures 1 to 3 , in one embodiment, the height of the overflow port 331 exceeds that of the substrate 320, so that when a certain amount of liquid accumulates in the extractor 310, it enters the overflow pipe 330 through the overflow port 331.

[0041] In this embodiment, the height of the overflow port 331 is higher than that of the substrate 320, so that the condensate in the extractor 310 needs to accumulate to a certain liquid level inside before it can enter the overflow pipe 330 through the overflow port 331 and flow back to the distribution pipe body 210. By setting the overflow port 331 at a position higher than the substrate 320, a liquid level control structure is formed, ensuring that the condensate does not immediately flow into the distribution pipe body 210, but stays in the extractor 310 for a period of time and is discharged through the overflow port 331 after accumulating to the set height.

[0042] The technical effect brought by this structure is that it can effectively control the flow rate and velocity of the reflux liquid, so that the contact between the liquid and the gas is more uniform and stable. The retention of the reflux liquid not only helps to further condense the residual light components in the extractor 310, but also avoids the disturbance of the gas-liquid contact state in the lower distribution pipe body 210 caused by the fluctuation of the condensate. At the same time, the reflux only occurs when the liquid level reaches the height of the overflow port 331, which can also avoid the direct short-circuit reflux of the liquid, enhancing the controllability of the device operation and the stability of the rectification separation. Therefore, this embodiment realizes a more efficient and controllable condensate reflux by controlling the overflow liquid level, which helps to improve the separation accuracy of the light and heavy components in the precursor.

[0043] Refer to Figures 1 to 3 , in one embodiment, the overflow pipe 330 is coaxially arranged with the connection hole 220, the inner diameter of the overflow pipe 330 is not less than the diameter of the connection hole 220, and the liquid in the overflow pipe 330 flows back into the rectification tower through the connection hole 220.

[0044] In this embodiment, the overflow pipe 330 is coaxially arranged with the connection hole 220, and the inner diameter of the overflow pipe 330 is not less than the diameter of the connection hole 220, so that the liquid in the overflow pipe 330 can smoothly flow back into the rectification tower through the connection hole 220. This structural design has a clear guiding effect. By the coaxial arrangement, the straightening and centering of the reflux path can be realized, which helps to improve the stability and efficiency of the liquid reflux.

[0045] Since the liquid in the overflow pipe 330 directly flows back into the rectification tower through the connection hole 220, it avoids the liquid accumulation or flow resistance that may be caused by the intermediate redundant flow channels or bends, thus ensuring that the condensate can flow back quickly and smoothly after reaching the liquid level of the overflow port 331. In addition, the inner diameter of the overflow pipe 330 is not less than the diameter of the connection hole 220, achieving full coverage of the connection hole 220 and improving the flushing effect.

[0046] Through this structural arrangement, the efficient and smooth reflux of the condensate can be realized, which helps to timely bring the heavy components entrained in the steam back to the rectification tower for re-separation, thereby improving the separation accuracy and stabilizing the material composition in the tower, and finally achieving the technical effect of reducing the light component content in the precursor and improving the product purity.

[0047] Refer to Figure 2 In one embodiment, a first flange 230 for connecting to a distillation column is provided at the bottom of the distribution tube body 210, and the connection holes 220 are provided on the first flange 230.

[0048] In this embodiment, a first flange 230 for connecting to a distillation column is provided at the bottom of the distribution tube body 210, and the connection holes 220 are provided on the first flange 230. By integrating the connection holes 220 at the position of the first flange 230, not only a compact integration in structure is achieved, but also it helps to improve the installation docking and sealing performance of the device.

[0049] As the connection interface between the distribution tube body 210 and the distillation column, the first flange 230 enables the entire distribution assembly 200 to be conveniently docked with the distillation column through a standard flange structure, simplifies the assembly process, and enhances the structural stability and maintainability. The connection holes 220 are located on the first flange 230, ensuring that the steam from the distillation column can directly enter the interior of the distribution tube body 210 from bottom to top, thereby realizing the direct contact and exchange between the steam and the condensate.

[0050] This design not only improves the sealing reliability of the connection part and avoids steam leakage, but also makes the structural relationship between the steam channel and the liquid return path clearer and the flow smoother, which is beneficial to maintaining the stability of the system operation and the continuity of the separation process. Therefore, through the integrated design of the flange structure and the connection holes 220 in this embodiment, while ensuring the stable connection of the device, it also further optimizes the steam transmission and liquid return paths, thereby helping to improve the overall distillation efficiency and product quality.

[0051] Refer to Figures 2 to 3 In one embodiment, an air outlet hole 341 is opened at one end of the gas-phase flow-through pipe 340 extending into the extractor 310, and an air inlet hole 342 is provided at the other end of the gas-phase flow-through pipe 340, and the air inlet hole 342 is flush with the bottom surface of the substrate 320.

[0052] In this embodiment, an air outlet hole 341 is opened at one end of the gas-phase flow-through pipe 340 extending into the extractor 310 for introducing the gas-phase substance from the distribution tube body 210 into the extractor 310; an air inlet hole 342 is provided at the other end of the gas-phase flow-through pipe 340, and the air inlet hole 342 is flush with the bottom surface of the substrate 320. This structural design optimizes the flow path and transmission efficiency of the gas phase, thereby further enhancing the effect of gas-liquid separation and component control.

[0053] The intake hole 342 is flush with the bottom surface of the substrate 320, which means that during the process of the steam rising from the distribution pipe body 210, it can directly enter the gas-phase flow pipe 340 without detouring or overcoming an additional structural height difference, which is beneficial to reducing the gas flow resistance and maintaining the smoothness of the gas-phase flow. At the same time, the outlet hole 341 is arranged at one end extending into the extractor 310, so that the steam can be dispersed and discharged after entering the extractor 310, further promoting the heat and mass exchange with the condensed liquid inside the extractor 310.

[0054] This structure not only helps to uniformly introduce the gas phase and prevent local accumulation of steam, but also improves the uniformity of the gas-phase distribution inside the extractor 310, making the condensation process more sufficient. In this way, the light components can smoothly enter the extractor 310 through the gas-phase flow pipe 340, while the heavy components are brought back to the distribution pipe body 210 during the contact with the condensed liquid and return to the distillation column with the liquid. Therefore, through the optimization of the structures at both ends of the gas-phase flow pipe 340 in this embodiment, the smooth conduction of the gas-phase path and the improvement of the condensation efficiency are realized, thereby enhancing the separation ability of the entire system for light and heavy components.

[0055] Refer to Figures 1 to 3 , in one embodiment, the distance from the overflow port 331 to the substrate 320 is less than the distance from the outlet hole 341 to the substrate 320.

[0056] In this embodiment, the distance from the overflow port 331 to the substrate 320 is less than the distance from the outlet hole 341 to the substrate 320, that is, the position of the overflow port 331 is relatively low, while the outlet hole 341 is located at a higher position. This structural layout forms a clear liquid-gas stratification control mechanism, further improving the stability and efficiency of gas-liquid separation and interaction.

[0057] Due to the lower position of the overflow port 331, the condensed liquid in the extractor 310 will reach the overflow port 331 first and flow back to the distribution pipe body 210 through the overflow pipe 330 during the process of the liquid level gradually rising. At the same time, the position of the outlet hole 341 is higher, so that the liquid accumulated in the extractor 310 will not submerge the outlet hole 341 under normal operating conditions, thus avoiding the problems of the gas-phase flow pipe 340 being blocked by liquid or the gas flow path being truncated.

[0058] This design ensures that while the reflux liquid is discharged in time, the steam from the distribution pipe body 210 can still be smoothly introduced into the extractor 310 through the gas-phase flow pipe 340, contact the condensation surface of the heat exchange component 100, and complete the enrichment process of the light components. At the same time, it also avoids the situation where the light components are "liquid-sealed" or cannot escape in time due to too high a liquid level. It can be seen that this structure realizes the effective separation and coordinated control of the gas-liquid paths in the height layout, which helps to further improve the condensation efficiency, separation accuracy, and the stability and reliability of the system operation.

[0059] In one embodiment, the substrate 320 and the side wall surface of the extractor 310 are integrally formed.

[0060] In this embodiment, the substrate 320 and the side wall surface of the extractor 310 are of an integrally formed structure, that is, the substrate 320 and the housing of the extractor 310 connected thereto are integrally formed through an integral manufacturing process. This structural design has significant advantages in terms of mechanical strength, sealing performance, and manufacturing simplification.

[0061] Firstly, integral forming avoids connection gaps that may be brought about by welding, screwing, or other assembly methods, reducing the risk of liquid or gas leakage at the source and enhancing the sealing and stability inside the extractor 310. Secondly, the overall structure eliminates the stress concentration problem at the structural connection, enhancing the ability of the entire device to resist thermal expansion and contraction, corrosion, and pressure during long-term operation, and is particularly suitable for high-temperature, high-humidity, or corrosive working conditions that may exist during the rectification process.

[0062] In addition, since the substrate 320 undertakes the function of supporting key components such as the overflow pipe 330 and the gas-phase circulation pipe 340, the integrated forming structure can also improve the installation accuracy of internal components, ensure the symmetry of the gas-liquid channel arrangement and the rationality of the flow path, and contribute to the uniform distribution and efficient contact of gas and liquid. In summary, this embodiment improves the structural strength, sealing reliability, and manufacturing consistency through the integral forming process, thereby further ensuring the safety, stability, and rectification effect of the entire semiconductor precursor rectification device during use.

[0063] Refer to Figure 2 , in one embodiment, a second flange 350 is provided on the outer side wall surface of the bottom of the liquid collection assembly 300, the second flange 350 protrudes from the outer side wall surface of the liquid collection assembly 300, a third flange 240 is provided on the outer side wall surface of the top of the distribution assembly 200, the third flange 240 protrudes from the outer side wall surface of the distribution assembly 200, and the second flange 350 and the third flange 240 are of the same diameter and are connected in cooperation to connect the liquid collection assembly 300 and the distribution assembly 200.

[0064] In this embodiment, a second flange 350 is provided on the outer side wall surface of the bottom of the liquid collection assembly 300, a third flange 240 is provided on the outer side wall surface of the top of the distribution assembly 200, and both are structures that protrude from their respective outer side wall surfaces. The second flange 350 and the third flange 240 have the same diameter and are connected in cooperation, thereby realizing the reliable connection between the liquid collection assembly 300 and the distribution assembly 200.

[0065] This flange connection structure has various technical effects. First, by setting the second flange 350 and the third flange 240 with equal diameters, it is convenient for standard docking between two components, improving the convenience and interchangeability of assembly. The use of the flange structure can ensure a high sealing performance when the two components are connected, effectively preventing the leakage of gas or condensate, and enhancing the safety and stability of the device operation.

[0066] Secondly, the convex setting of the flange makes the connection part have a larger stress area, thereby enhancing the connection strength. During actual operation, it can better withstand internal pressure fluctuations or mechanical vibrations, reducing the risk of failures during the use of the device. In addition, the flange connection method is also convenient for disassembly and maintenance, facilitating the cleaning, replacement, or overhaul of internal structures such as the substrate 320, the overflow pipe 330, the gas-phase flow pipe 340, etc., which is beneficial to the long-term stable operation and maintenance management of the device.

[0067] Refer to Figure 4 , in one embodiment, it further includes a first temperature control component 400. The first temperature control component 400 includes a heating pipeline 410 arranged inside the side wall of the extractor 310. The heating pipeline 410 is wound around the inside of the side wall of the extractor 310. The top of the heating pipeline 410 is flush with the top of the overflow pipe 330 and is connected to a heat source device for heating the liquid inside the extractor 310. The first temperature control component 400 further includes a first temperature sensor for collecting the temperature of the liquid inside the extractor 310.

[0068] In this embodiment, this structure dynamically regulates the temperature of the condensate inside the extractor 310, further optimizing the gas-liquid contact conditions and separation effect. Specifically, the setting of the heating pipeline 410 can provide heat compensation when the liquid temperature is too low, raising the temperature of the condensate. In this way, when the steam from the distillation column contacts the reflux condensate inside the distribution pipe body 210, due to the higher liquid temperature, the possibility of secondary condensation of the light components during the contact can be effectively reduced, avoiding the light components being brought back to the bottom of the column, thereby improving the removal efficiency of the light components during the distillation process.

[0069] In addition, the setting of the first temperature sensor enables the system to monitor the temperature state of the liquid inside the extractor 310 in real time and adjust the heating intensity of the heating pipeline 410 accordingly, realizing the closed-loop control of the liquid temperature. This intelligent temperature control design helps the system maintain the best gas-liquid balance state under different working conditions, further enhancing the effective separation of light and heavy components by the device.

[0070] In one embodiment, it further includes a second temperature control component. The second temperature control component is connected to the overflow pipe 330 and is used to heat the liquid inside the overflow pipe 330.

[0071] In this embodiment, the overflow pipe 330 serves as an important channel for the condensate to flow back from the extractor 310 to the distribution pipe body 210 and finally enter the rectification column. The temperature of the liquid inside it will directly affect the mass transfer and heat exchange state when contacting the steam. By setting a heating function in the overflow pipe 330, the second temperature control component can prevent the premature condensation of light components caused by too low liquid temperature, thereby avoiding the light components being brought back to the bottom of the rectification column by the liquid, ensuring that the light components fully enter the extractor 310 and then enter the heat exchange component 100, and improving the separation efficiency.

[0072] Referring to Figures 2 to 3 , in one embodiment, the air outlet 341 is arranged on the side wall surface of the overflow pipe 330 away from the substrate 320, and the top end surface of the gas-phase flow pipe 340 away from the substrate 320 is closed.

[0073] In this embodiment, the closed top end surface means that after the steam enters the gas-phase flow pipe 340, it cannot be directly discharged in the vertical direction, but must turn and escape from the air outlet 341 on the side wall. The air outlet 341 is arranged in the area close to the overflow pipe 330, so that the steam finally discharges from the side wall close to the liquid return path, which is beneficial to the more uniform distribution of the steam in the extractor 310, and at the same time avoids the air flow directly impacting the top area of the extractor 310 and maintains the stability of the internal gas phase environment. In addition, the top closed structure also has the function of preventing the liquid from entering the gas-phase flow pipe 340 from the upper end, further ensuring the purity and smoothness of the gas-phase path and preventing gas-liquid cross-contamination.

[0074] Referring to Figures 1 to 3 , in one embodiment, a sampling outlet 360 is provided on the liquid collection assembly 300. The sampling outlet 360 is arranged on the side wall surface of the extractor 310 close to the substrate 320. The distance from the sampling outlet 360 to the substrate 320 is less than the distance from the overflow port 331 to the substrate 320, and a concentration sensor 370 is provided on the sampling outlet 360.

[0075] In this embodiment, the sampling outlet 360 is arranged at a position lower than the overflow port 331, so that it can start sampling before the condensate reaches the overflow liquid level, thereby reflecting the actual concentration change trend of the liquid at the bottom of the extractor 310 earlier and more accurately. Since the heavy components are preferentially condensed and collected at the bottom of the extractor 310, the liquid sample obtained by the sampling outlet 360 can more truly reflect the proportion of the remaining light components in the condensate.

[0076] The concentration sensor 370 is arranged on the sampling outlet 360, and can perform real-time online monitoring on the liquid flowing through this position, and accurately detect the concentration change of the light components in the liquid. When the sensor detects that the concentration reaches the preset threshold, a signal can be sent in combination with the control system, which is used to judge whether the liquid precursor in the rectification column has completed light component removal, or as a basis for adjusting the operating states of various components of the system (such as temperature control, condensation, reflux, etc.).

[0077] An embodiment of the present invention further provides a precursor rectification system for semiconductors, including the above-mentioned precursor rectification device for semiconductors, characterized in that it further includes a rectification column, and the rectification column is connected to the distribution component 200.

[0078] In this embodiment, the rectification column serves as a preliminary separation site for the raw material gas. Through the multi-stage mass transfer process inside the column, the light and heavy components are preliminarily separated. The rising steam separated is introduced into the interior of the distribution component 200 via a connection structure (such as the connection hole 220 provided on the first flange 230). In the distribution component 200, the steam further contacts the condensate refluxed from the liquid collection component 300, realizing the re-capture and reflux of the heavy components to ensure that they are brought back into the rectification column for secondary rectification; at the same time, the light components continue to rise because they are not condensed, realizing final enrichment and discharge.

[0079] An embodiment of the present invention further provides a precursor rectification method for semiconductors, using the above-mentioned precursor rectification system for semiconductors, characterized in that it includes the following steps: Adjust the temperature of the rectification column to the evaporation temperature T1, where T1 is between the boiling point Ta of the heavy component A and the boiling point Tb of the light component B in the liquid precursor inside the rectification column.

[0080] Adjust the heat exchange component 100 to the condensation temperature T2, where T2 is less than Tb, and collect the liquid generated by the condensation of the heat exchange component 100 until the liquid accumulates in the extractor 310 and flows into the overflow pipe 330.

[0081] Adjust the first temperature adjustment component 400 until the temperature of the liquid in the extractor 310 reaches T3, where T3 is Tb * floating coefficient K1.

[0082] Adjust the second temperature adjustment component until the temperature of the liquid in the overflow pipe 330 reaches T4, where T4 is Tb * floating coefficient K2.

[0083] Continuously evaporate until the concentration of the light component B in the liquid in the extractor 310 reaches the threshold, and judge that the liquid precursor in the rectification column has completed light component removal.

[0084] In this embodiment, first, by heating the rectification column, the temperature inside the column is adjusted to the evaporation temperature T1, which is set between the boiling point Ta of the heavy component A and the boiling point Tb of the light component B, so that the heavy component A in the liquid precursor remains in a liquid state, while the light component B is converted into steam and enters the upper space, thus forming a preliminary separation of the light and heavy components.

[0085] Subsequently, the heat exchange component 100 is adjusted to the condensation temperature T2, where T2 is lower than the boiling point Tb of the light component B, such that a portion of the vapor condenses on the surface of the heat exchange component 100. The condensate converges and flows into the extractor 310, and reflux is achieved through the overflow pipe 330. During the contact process between this condensate, acting as a "rinsing liquid", and the vapor from the rectification column, it can effectively adsorb and carry the heavy components entrained in the vapor, causing them to re-enter the rectification column for reprocessing, thereby reducing the possibility of heavy components being carried out during the distillation process and improving the separation accuracy.

[0086] Next, by adjusting the first temperature control component 400, the temperature of the liquid in the extractor 310 is increased to T3, where T3 is Tb multiplied by the floating coefficient K1. Then, by adjusting the second temperature control component, the temperature of the liquid in the overflow pipe 330 is increased to T4, where T4 is Tb multiplied by the floating coefficient K2. Both T3 and T4 are between the boiling point Ta of the heavy component A and the boiling point Tb of the light component B. The role of the first and second temperature control components is to heat the condensate to maintain it at a temperature level close to or higher than the boiling point of the light component while less than the boiling point of the heavy component, thereby reducing the probability of the light component B being condensed during the contact with the reflux liquid or flowing through the overflow pipe 330, effectively avoiding ineffective reflux and loss of light components, and improving the light component removal efficiency.

[0087] Finally, through continuous evaporation operation and monitoring the concentration of the light component B in the liquid in the extractor 310, when it reaches the set threshold, it is determined that the liquid precursor in the rectification column has completed the light component removal process.

[0088] In summary, the core technical effect of this method lies in utilizing the rinsing effect of high-temperature condensate on the vapor to effectively recover the heavy components entrained in the vapor, and controlling the temperature of the reflux liquid through the temperature control components to avoid premature condensation of the light components, thereby achieving efficient and precise separation of light and heavy components, and significantly improving the purity and process adaptability of the semiconductor precursor.

[0089] The technical features of the above-described embodiments can be combined arbitrarily. For the sake of brevity of description, not all possible combinations of the technical features in the above-described embodiments are described. However, as long as there is no contradiction in the combination of these technical features, it should be considered as within the scope described in this specification.

[0090] The above-described embodiments merely represent several implementation manners of the present invention. Their descriptions are relatively specific and detailed, but they should not be construed as limiting the scope of the invention patent. It should be noted that for those of ordinary skill in the art, without departing from the concept of the present invention, several modifications and improvements can be made, and these all belong to the protection scope of the present invention. Therefore, the protection scope of the present invention patent shall be subject to the appended claims.

Claims

1. A precursor rectification device for semiconductors, comprising a heat exchange component (100), characterized in that, Further comprising: A distribution component (200), the distribution component (200) includes a distribution pipe body (210), and a connection hole (220) for the rectifying column to convey steam is provided at the bottom of the distribution pipe body (210); A liquid collecting component (300) disposed between the distribution pipe body (210) and the heat exchange component (100), the liquid collecting component (300) includes a sampler (310) for collecting the liquid condensed by the heat exchange component (100), a substrate (320) is provided at the bottom of the sampler (310), an overflow pipe (330) and a plurality of gas-phase flow pipes (340) are arranged on the substrate (320), and the gas-phase flow pipes (340) communicate the sampler (310) with the distribution pipe body (210); one end of the overflow pipe (330) extends into the sampler (310) to form a liquid collecting space (380) with the side wall surface of the sampler (310), an overflow port (331) is provided at the end of the overflow pipe (330) extending into the sampler (310), and the other end extends into the distribution component (200) and is located above the connection hole (220), so that the condensed liquid can contact the steam coming out of the rectifying column in the distribution pipe body (210) to wash the heavy component substances in the steam.

2. The semiconductor precursor rectification device according to claim 1, wherein The overflow pipe (330) is located at the central position of the substrate (320), and a plurality of the gas-phase flow pipes (340) are arranged around the overflow pipe (330).

3. The semiconductor precursor rectification device according to claim 1, wherein The height of the overflow port (331) exceeds that of the substrate (320), so that when a certain amount of liquid accumulates in the sampler (310), it enters the overflow pipe (330) through the overflow port (331).

4. The semiconductor precursor rectification device according to claim 1, characterized in that, The overflow pipe (330) and the connection hole (220) are coaxially arranged, the inner diameter of the overflow pipe (330) is not less than the diameter of the connection hole (220), and the liquid in the overflow pipe (330) flows back into the rectifying column through the connection hole (220).

5. The semiconductor precursor rectification device according to claim 1, characterized in that, A first flange (230) for connecting the rectifying column is provided at the bottom of the distribution pipe body (210), and the connection hole (220) is arranged on the first flange (230).

6. The rectification device for semiconductor precursors according to claim 1, characterized in that, An air outlet hole (341) is opened at one end of the gas-phase flow pipe (340) extending into the sampler (310), and an air inlet hole (342) is provided at the other end of the gas-phase flow pipe (340), and the air inlet hole (342) is flush with the bottom surface of the substrate (320).

7. The semiconductor precursor rectification device according to claim 6, characterized in that, The distance from the overflow port (331) to the substrate (320) is less than the distance from the air outlet hole (341) to the substrate (320).

8. The semiconductor precursor rectification device according to claim 1, characterized in that, The substrate (320) and the side wall surface of the sampler (310) are integrally formed.

9. The semiconductor precursor rectification device according to claim 1, wherein, A second flange (350) is provided on the outer side wall surface at the bottom of the liquid collecting assembly (300). The second flange (350) protrudes from the outer side wall surface of the liquid collecting assembly (300). A third flange (240) is provided on the outer side wall surface at the top of the distribution assembly (200). The third flange (240) protrudes from the outer side wall surface of the distribution assembly (200). The second flange (350) and the third flange (240) have the same diameter and are connected in cooperation to connect the liquid collecting assembly (300) and the distribution assembly (200).

10. The semiconductor precursor rectification device according to claim 1, wherein It further includes a first temperature regulating assembly (400). The first temperature regulating assembly (400) includes a heating pipeline (410) provided inside the side wall of the extractor (310). The heating pipeline (410) is wound inside the side wall of the extractor (310). The top of the heating pipeline (410) is flush with the top of the overflow pipe (330) and is connected to a heat source device for heating the liquid inside the extractor (310). The first temperature regulating assembly (400) further includes a first temperature sensor for collecting the temperature of the liquid inside the extractor (310).

11. The semiconductor precursor rectification device according to claim 1, wherein It further includes a second temperature regulating assembly which is connected to the overflow pipe (330) for heating the liquid inside the overflow pipe (330).

12. The semiconductor precursor rectification device according to claim 6, wherein The air outlet hole (341) is provided on the side wall surface of the overflow pipe (330) on the side away from the substrate (320). The top end surface on the side away from the substrate (320) of the gas phase flow pipe (340) is closed.

13. The semiconductor precursor rectification device according to claim 1, wherein A liquid extraction port (360) is provided on the liquid collecting assembly (300). The liquid extraction port (360) is provided on the side wall surface inside the extractor (310) close to the substrate (320). The distance from the liquid extraction port (360) to the substrate (320) is less than the distance from the overflow port (331) to the substrate (320). A concentration sensor (370) is provided on the liquid extraction port (360).

14. A precursor rectification system for semiconductors, comprising the precursor rectification device for semiconductors according to any one of claims 1-13, characterized in that, It further includes a rectification column which is connected to the distribution assembly (200).

15. A rectification method for semiconductor precursors, using the semiconductor precursor rectification system described in claim 14, characterized in that, It includes the following steps: Adjust the temperature of the rectification column to the evaporation temperature T1, where T1 is between the boiling point Ta of the heavy component A and the boiling point Tb of the light component B in the liquid precursor inside the rectification column; Adjust the heat exchange assembly (100) to the condensation temperature T2, where T2 is less than Tb. Collect the liquid condensed by the heat exchange assembly (100) until the liquid accumulates in the extractor (310) and flows into the overflow pipe (330); Adjust the first temperature regulating assembly (400) until the temperature of the liquid inside the extractor (310) reaches T3, where T3 is Tb * floating coefficient K1; Adjust the second temperature regulating assembly until the temperature of the liquid inside the overflow pipe (330) reaches T4, where T4 is Tb * floating coefficient K2; Continuously evaporate until the concentration of the light component B in the liquid inside the extractor (310) reaches the threshold value, and judge that the liquid precursor inside the rectification column has completed light component removal.

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