A semiconductor precursor distillation device, system and method

Abstract

The present invention discloses a semiconductor precursor distillation device, system and method, including a heat exchange component, a distribution component and a liquid collecting component, wherein the distribution component includes a distribution pipe body, and the bottom of the distribution pipe body is provided with a connection hole for conveying steam to a distillation tower; the liquid collecting component is placed between the distribution pipe body and the heat exchange component, and includes an extractor for collecting liquid generated by condensation of the heat exchange component, the bottom of the extractor is provided with a base plate, an overflow pipe and a plurality of gas phase flow pipes are provided on the base plate, and the gas phase flow pipes connect 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 extends into the distribution component and is located above the connection hole, so that the condensed liquid can contact with the steam coming out of the distillation tower in the distribution pipe body, thereby flushing the heavy component substances in the steam, and then reflux to the distillation tower together, so that the corresponding light component substances can be quickly enriched and discharged in time, so that the content of 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 in particular to a semiconductor precursor distillation device, system and method. Background Art

[0002] As semiconductor manufacturing processes advance toward 5nm technology nodes and below, the preparation of high-purity semiconductor precursors (such as metal organics and halides) has become a key challenge. The purity of semiconductor precursors directly impacts chip performance and reliability. In particular, residual metal impurities, oxygen-containing contaminants, and particulate matter must be controlled at the ppb (parts per billion) level, placing near-limited demands on traditional chemical distillation technology. However, the purification scenarios for semiconductor precursors differ significantly from those in the traditional chemical industry: the former requires small-batch, high-precision impurity separation, while the latter typically focuses on large-scale continuous production. Traditional chemical distillation typically processes tons of material and allows for large composition fluctuations, while precursor distillation requires ppb-level impurity control at kilogram-level operating volumes, making the two difficult to reconcile in terms of process design logic.

[0003] Patent CN201384866Y provides a vertical automatic reflux extraction and distillation device. The device consists of a mist trap, a shell and tube condenser, a reflux extraction controller, a tower top extraction port, a distillation tower, an extraction flowmeter, an extraction regulating valve, and a tower bottom reboiler. The material evaporates in the tower bottom reboiler, and after heat and mass transfer inside the tower, the material vapor enters the tower top shell and tube condenser, condenses, and falls into the sump of the reflux extraction controller; the condensed liquid enters the annular sump from both ends of the sump, and some is redistributed and refluxed through the overflow holes on the side of the overflow weir, some is distributed through the tear holes, and some is extracted from the tower top extraction port through the flowmeter and regulating valve. The non-condensable gas is removed from the tower top vacuum port after the droplets are removed by the mist trap.

[0004] However, despite widespread use in the traditional chemical industry, the vertical automatic reflux extraction distillation apparatus provided by the aforementioned patent has exposed a series of limitations in the purification of semiconductor precursors. First, the theoretical number of plates and separation efficiency of traditional apparatuses are insufficient to meet the separation requirements of light and heavy components with similar boiling points. This results in impurity residues far exceeding semiconductor process requirements, and separation efficiency is difficult to improve. Summary of the Invention

[0005] Based on this, it is necessary to provide a semiconductor precursor distillation device, system and method to address the above-mentioned problem of insufficient gas-liquid phase separation.

[0006] The present application provides a semiconductor precursor distillation device, comprising a heat exchange component and further comprising:

[0007] A distribution assembly, the distribution assembly comprising a distribution pipe body, the bottom of the distribution pipe body being provided with a connection hole for conveying steam to the distillation tower;

[0008] A liquid collecting assembly is placed between the distribution pipe body and the heat exchange assembly, and the liquid collecting assembly includes an extractor for collecting the liquid generated by condensation of the heat exchange assembly. A base plate is provided at the bottom of the extractor, and an overflow pipe and a plurality of gas flow pipes are provided on the base plate. The gas flow pipes connect the extractor and the distribution pipe body; one end of the overflow pipe extends into the extractor to form a liquid collecting space with the side wall of the extractor, and an overflow port is provided on the end of the overflow pipe extending into the extractor, and the other end extends into the distribution assembly and is located above the connecting hole, so that the condensed liquid can contact the steam coming out of the distillation tower in the distribution pipe body, thereby flushing the heavy components in the steam.

[0009] Optionally, the overflow pipe is located at the center of the substrate, and a plurality of the gas flow pipes are arranged around the overflow pipe.

[0010] Optionally, the overflow port is located at a height exceeding the base plate, so that when a certain amount of liquid accumulates in the extractor, it flows into the overflow pipe through the overflow port.

[0011] Optionally, the overflow pipe is coaxially arranged with the connecting hole, the inner diameter of the overflow pipe is not less than the diameter of the connecting hole, and the liquid in the overflow pipe flows back into the distillation tower through the connecting hole.

[0012] Optionally, a first flange for connecting to a distillation tower is provided at the bottom of the distribution pipe body, and the connecting hole is provided on the first flange.

[0013] Optionally, an air outlet is formed at one end of the gas phase circulation pipe extending into the extractor, and an air inlet is formed at the other end of the gas phase circulation pipe, and the air inlet is flush with the bottom surface of the substrate.

[0014] Optionally, the distance from the overflow port to the substrate is smaller than the distance from the air outlet to the substrate.

[0015] Optionally, the base plate and the side wall surface of the extractor are integrally formed.

[0016] Optionally, a second flange is provided on the outer wall surface of the bottom of the liquid collection component, and the second flange protrudes from the outer wall surface of the liquid collection component. A third flange is provided on the outer wall surface of the top of the distribution component, and the third flange protrudes from the outer wall surface of the distribution component. The second flange and the third flange have the same diameter and are matched to connect the liquid collection component and the distribution component.

[0017] Optionally, it further includes a first temperature control component, which includes a heating pipeline arranged in the side wall of the extractor, the heating pipeline is wound in 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 in the extractor. The first temperature control component also includes a first temperature sensor for collecting the temperature of the liquid in the extractor.

[0018] Optionally, a second temperature adjustment component is further included, which is connected to the overflow pipe and is used to heat the liquid in the overflow pipe.

[0019] Optionally, the gas outlet is provided on a side wall surface of the overflow pipe away from the substrate, and a top end surface of the gas phase flow pipe away from the substrate is closed.

[0020] Optionally, the liquid collecting assembly is provided with a collection outlet, which is arranged on the side wall surface of the extractor close to the substrate, the distance from the collection outlet to the substrate is smaller than the distance from the overflow port to the substrate, and the collection outlet is provided with a concentration sensor.

[0021] The present application also provides a semiconductor precursor distillation system, comprising the above-mentioned semiconductor precursor distillation device, and also comprising a distillation tower, wherein the distillation tower is connected to the distribution component.

[0022] Compared with the existing technology, the technical solution provided by this application has the following beneficial effects:

[0023] The connection hole at the bottom of the distribution tube body is connected to the steam outlet of the distillation tower, allowing the rising steam to diffuse along the internal space of the distribution tube body. The extractor of the liquid collection assembly is connected to the distribution tube body through a gas flow pipe on the base plate. Steam flows vertically upward through the gas flow pipe into the space above the extractor and is further transported to the heat exchange component for condensation. During this process, the condensed liquid collected in the extractor flows in the opposite direction through the overflow pipe below the base plate. One end of the overflow pipe extends into the distribution tube body, and its overflow port is higher than the connection hole. This allows the reflux liquid to flow from top to bottom in the distribution tube body, forming countercurrent contact with the newly rising steam entering through the connection hole. The condensate has a scouring effect on the incompletely vaporized heavy component droplets or high-boiling point substances entrained in the steam, forcing the heavy components to flow back to the distillation tower with the liquid to re-participate in the distillation. The light components in the steam, due to the difference in boiling point, enter the heat exchange component through the gas flow pipe. The uniform arrangement of the gas phase circulation tubes on the substrate not only ensures the uniform distribution of steam flow, but also prevents the liquid from flowing back into the distribution pipe body when the steam pressure fluctuates through the physical barrier effect of the substrate on the liquid in the extractor. 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 condensate exceeds the height of the overflow port, the excess liquid is automatically discharged through the overflow pipe, which not only maintains the dynamic update of the light component condensate in the extractor, but also prevents the gas phase circulation tube from being blocked by liquid due to excessive liquid level. The continuous condensation of the light component steam by the heat exchange component and the collection and discharge of the extractor form a closed loop, so that the light component substances are continuously concentrated and discharged from the system, while the heavy components are intercepted and returned to the distillation tower through gas-liquid countercurrent contact, reducing the enrichment of the heavy components at the top of the distillation tower, and ultimately achieving the efficient removal of light component impurities in the semiconductor precursor and the cyclic purification of the heavy components, thereby improving the separation efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 A cross-sectional structural diagram of a semiconductor precursor distillation device provided in one embodiment of the present application;

[0025] Figure 2 A cross-sectional structural diagram of a liquid collecting component and a distribution component of a semiconductor precursor distillation device provided in one embodiment of the present application;

[0026] Figure 3 A structural diagram of a liquid collecting assembly of a semiconductor precursor distillation device provided in one embodiment of the present application;

[0027] Figure 4 A schematic diagram of a first temperature adjustment component of a semiconductor precursor distillation device provided in one embodiment of the present application;

[0028] Figure 5 This is an external structural diagram of a semiconductor precursor distillation device provided in one embodiment of the present application.

[0029] Description of reference numerals:

[0030] 100, heat exchange component; 200, distribution component; 210, distribution pipe body; 220, connecting hole; 230, first flange; 240, third flange; 300, liquid collection component; 310, extractor; 320, base plate; 330, overflow pipe; 331, overflow port; 340, gas flow pipe; 341, air outlet; 342, air inlet; 350, second flange; 360, extraction port; 370, concentration sensor; 380, liquid collection space; 400, first temperature control component; 410, heating pipeline. DETAILED DESCRIPTION

[0031] To make the above-mentioned objects, features, and advantages of the present invention more readily apparent, specific embodiments of the present invention are described in detail below with reference to the accompanying drawings. The following description sets forth numerous specific details to facilitate a full understanding of the present invention. However, the present invention can be implemented in many other ways than those described herein, and those skilled in the art may make similar modifications without departing from the scope of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed below.

[0032] In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise", "axial", "radial", "circumferential" and the like to indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are 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, and therefore should not be understood as limiting the present invention.

[0033] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of the technical features being referred to. Thus, a feature defined as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of the present invention, "plurality" means at least two, such as two, three, etc., unless otherwise specifically defined.

[0034] In the present invention, unless otherwise specified or limited, the terms "installed," "connected," "connect," "fixed," etc. should be understood in a broad sense. For example, they can refer to fixed connection, detachable connection, or integration; mechanical connection, electrical connection; direct connection, or indirect connection through an intermediate medium; internal communication between two components, or interaction between two components, unless otherwise specified. Those skilled in the art will understand the specific meanings of the above terms in the present invention based on specific circumstances.

[0035] See Figures 1 to 3 One embodiment of the present invention provides a semiconductor precursor distillation device, comprising a heat exchange component 100, and further comprising:

[0036] The distribution assembly 200 includes a distribution pipe body 210 , and a connection hole 220 for delivering steam to the distillation tower is provided at the bottom of the distribution pipe body 210 ;

[0037] The liquid collecting assembly 300 is placed between the distribution pipe body 210 and the heat exchange assembly 100. The liquid collecting assembly 300 includes a sampler 310 for collecting the liquid generated by the condensation of the heat exchange assembly 100. The bottom of the sampler 310 is provided with a base plate 320. The base plate 320 is provided with an overflow pipe 330 and a plurality of gas phase flow pipes 340. The gas phase flow pipes 340 connect the sampler 310 with the distribution pipe body 210. One end of the overflow pipe 330 extends into the sampler 310 and forms a liquid collecting surface with the side wall of the sampler 310. In the space 380, an overflow port 331 is provided on one end of the overflow pipe 330 extending into the extractor 310, and the other end extends into the distribution component 200 and is located above the connecting hole 220, so that the condensed liquid can contact the steam coming out of the distillation tower in the distribution pipe body 210, thereby flushing the heavy component substances in the steam, and then reflux them into the distillation tower together. The corresponding light component substances can be quickly enriched and discharged in time, so that the content of light component substances in the semiconductor precursor is reduced.

[0038] See Figure 2 In the figure, the descending arrow is the liquid produced by condensation, the ascending arrow is the steam produced by the distillation tower, and the dotted box area is the area where the condensed liquid contacts the steam and produces a flushing effect.

[0039] In this embodiment, the connection hole 220 at the bottom of the distribution pipe body 210 is connected to the steam outlet of the distillation tower, allowing the rising steam to diffuse along the internal space of the distribution pipe body 210. The extractor 310 of the liquid collection assembly 300 is connected to the distribution pipe body 210 through the gas phase circulation pipe 340 on the base plate 320 to form a gas path. The steam enters the top space of the extractor 310 vertically upward through the gas phase circulation 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 in the opposite direction through the overflow pipe 330 below the base plate 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. This allows the reflux liquid to form countercurrent contact with the new rising steam entering from the connection hole 220 when flowing from top to bottom in the distribution pipe body 210. The condensate flushes the incompletely vaporized heavy component droplets or high-boiling-point substances entrained in the steam, forcing the heavy components to flow back into the distillation tower with the liquid to re-participate in the distillation. The light components in the steam, due to the difference in boiling points, enter the heat exchange assembly 100 through the gas-phase flow tube 340. The uniform arrangement of the gas-phase flow tube 340 on the base plate 320 not only ensures uniform distribution of the steam flow, but also, through the physical barrier effect of the base plate 320 on the liquid in the extractor 310, prevents the liquid from flowing back into the distribution pipe 210 when the steam pressure fluctuates. 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 condensate exceeds the height of the overflow port 331, the excess liquid is automatically discharged through the overflow pipe 330. This not only maintains the dynamic renewal of the light component condensate in the extractor 310, but also prevents the gas-phase flow tube 340 from being blocked by liquid due to excessive liquid level. The continuous condensation of light component steam by the heat exchange component 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 and returned to the distillation tower through gas-liquid countercurrent contact, reducing the enrichment of the heavy components at the top of the distillation tower, and ultimately achieving efficient removal of light component impurities in the semiconductor precursor and cyclic purification of the heavy components, thereby improving separation efficiency.

[0040] In the existing technology, the condensate produced by the shell and tube condenser needs to be refluxed and extracted through a multi-stage distribution structure such as a guide tube, an overflow weir and a tear hole. Its separation efficiency is limited by the static overflow and passive diversion mechanism. For example, the overflow hole on the side of the overflow weir can only control the reflux volume through a fixed aperture. Although the capillary action of the tear hole can assist in liquid distribution, it is difficult to accurately adjust the extraction ratio of the light component. Especially when dealing with light and heavy component systems with similar boiling points and slight differences in physical properties, it is easy to cause secondary entrainment of the condensate or residual light components. In addition, although the mist collector can intercept droplets in the gas phase, it cannot actively retain the heavy component molecules that are not completely condensed in the steam, which ultimately makes it difficult for the light component content to exceed the 2% threshold.

[0041] Furthermore, the coordinated design of the gas-phase circulation tube 340 and the substrate 320 makes up for the defect of cross-interference of the gas-liquid path in the traditional device. The uniform arrangement of the gas-phase circulation tube 340 on the substrate 320 not only realizes the homogenized distribution of the steam flow, 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 the gas-liquid two-phase flow in the prior art. For example, although the structure of the guide tube and the tear hole 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 collecting tank, resulting in some light components being carried back to the tower by the reflux liquid. However, this embodiment ensures that the light component vapor reaches the condensation area directly under undisturbed conditions through the spatial isolation of the substrate 320 and the directional diversion of the gas-phase circulation tube 340, thereby realizing the rapid enrichment and directional discharge of the light component.

[0042] See Figures 1 to 3 In one embodiment, the overflow pipe 330 is located at the center of the substrate 320 , and a plurality of gas flow pipes 340 are disposed around the overflow pipe 330 .

[0043] In this embodiment, the overflow pipe 330 is located at the center of the base plate 320, and a plurality of gas-phase circulation pipes 340 are arranged around the overflow pipe 330. This structural arrangement further optimizes the contact path and contact efficiency between the liquid and the gas in the distribution pipe body 210. Specifically, the overflow pipe 330 in the center enables the condensed liquid collected in the extractor 310 to preferentially flow back from the central area to the distribution pipe body 210. At the same time, the structure surrounded by the gas-phase circulation pipes 340 arranged around it allows the steam from the distribution pipe body 210 to evenly rise from the periphery to the base plate 320 and enter the extractor 310 through the gas-phase circulation pipes 340 during the process of flowing to the extractor 310.

[0044] This uniform distribution from the center outward enables more complete and uniform contact between the gas and liquid phases within the distribution pipe 210, enhancing the condensate's ability to flush heavy components from the steam. Furthermore, this layout helps maintain the stability of gas-liquid flow within the device, avoiding localized turbulence or biased flow, thereby further improving the efficiency of the distillation process. Consequently, this structure more effectively recovers heavy components and enriches light components, helping to reduce the content of light components in the final product and enhance the purity of the semiconductor precursor.

[0045] See Figures 1 to 3 In one embodiment, the overflow port 331 is located at a height higher than the base plate 320 , so that when a certain amount of liquid accumulates in the extractor 310 , the liquid enters the overflow pipe 330 through the overflow port 331 .

[0046] In this embodiment, the overflow port 331 is located at a higher level than the base plate 320, so that the condensate in the extractor 310 must accumulate internally to a certain level before it can flow through the overflow port 331 into the overflow pipe 330 and back into the distribution pipe body 210. By placing the overflow port 331 at a position higher than the base plate 320, a liquid level control structure is formed, ensuring that the condensate does not immediately flow into the distribution pipe body 210. Instead, it remains in the extractor 310 for a period of time and accumulates to a set height before being discharged through the overflow port 331.

[0047] The technical effect brought about by this structure is that it can effectively control the flow rate and flow rate 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 by the fluctuation of the condensate. At the same time, reflux only occurs when the liquid level reaches the height of the overflow port 331, and direct short-circuit reflux of the liquid can also be avoided, thereby enhancing the controllability of the operation of the device and the stability of the distillation separation. Therefore, this embodiment achieves a more efficient and controllable reflux of the condensate by controlling the overflow liquid level, which helps to improve the separation accuracy of the light and heavy components in the precursor.

[0048] See Figures 1 to 3 In one embodiment, the overflow pipe 330 is coaxially arranged with the connecting hole 220 , and the inner diameter of the overflow pipe 330 is not less than the diameter of the connecting hole 220 . The liquid in the overflow pipe 330 flows back to the distillation tower through the connecting hole 220 .

[0049] In this embodiment, overflow pipe 330 is coaxially arranged with connecting hole 220, and the inner diameter of overflow pipe 330 is no less than the diameter of connecting hole 220, allowing liquid in overflow pipe 330 to smoothly flow back into the distillation column through connecting hole 220. This structural design has a clear flow-guiding effect. The coaxial arrangement can achieve a straight and centered reflux path, helping to improve the stability and efficiency of liquid reflux.

[0050] Because the liquid in overflow pipe 330 flows directly back to the distillation column through connecting hole 220, it avoids liquid accumulation or flow resistance caused by unnecessary intermediate flow channels or bends, ensuring that the condensate can flow back quickly and smoothly after reaching the liquid level of overflow port 331. Furthermore, the inner diameter of overflow pipe 330 is no smaller than the diameter of connecting hole 220, ensuring full coverage of connecting hole 220 and improving the flushing effect.

[0051] This structural arrangement enables efficient and smooth reflux of the condensate, helping to promptly bring the heavy components entrained in the steam back to the distillation tower for re-separation, thereby improving the separation accuracy and stabilizing the material composition in the tower, ultimately achieving the technical effect of reducing the content of light components in the precursor and improving product purity.

[0052] See Figure 2 In one embodiment, a first flange 230 for connecting to a distillation tower is provided at the bottom of the distribution pipe body 210 , and the connecting hole 220 is provided on the first flange 230 .

[0053] In this embodiment, the bottom of the distribution pipe body 210 is provided with a first flange 230 for connecting to the distillation column, and the connection hole 220 is provided on the first flange 230. By integrating the connection hole 220 at the position of the first flange 230, not only a compact structure is achieved, but also the installation and docking performance of the device are improved.

[0054] The first flange 230 serves as the interface between the distribution pipe body 210 and the distillation column. Its configuration allows the entire distribution assembly 200 to be easily docked with the distillation column using a standard flange structure, simplifying the assembly process and enhancing structural stability and maintainability. The connection hole 220 located on the first flange 230 ensures that steam from the distillation column can directly enter the distribution pipe body 210 from bottom to top, achieving direct contact and exchange between steam and condensate.

[0055] This design not only improves the sealing reliability of the connection and prevents steam leakage, but also clarifies the structural relationship between the steam channel and the liquid return path, ensuring smoother flow, thereby maintaining the stability of system operation and the continuity of the separation process. Therefore, through the integrated design of the flange structure and the connection hole 220, this embodiment not only ensures a stable connection of the device, but also further optimizes the steam transmission and liquid return path, thereby helping to improve overall distillation efficiency and product quality.

[0056] See Figures 2 to 3 In one embodiment, a gas outlet hole 341 is formed at one end of the gas flow pipe 340 extending into the extractor 310 , and a gas inlet hole 342 is formed at the other end of the gas flow pipe 340 , and the gas inlet hole 342 is flush with the bottom surface of the substrate 320 .

[0057] In this embodiment, one end of the gas flow tube 340 extending into the extractor 310 is provided with an outlet hole 341 for directing gaseous material from the distribution tube 210 into the extractor 310. The other end of the gas flow tube 340 is provided with an inlet hole 342, which is flush with the bottom surface of the base plate 320. This structural design optimizes the gas flow path and transmission efficiency, thereby further enhancing the gas-liquid separation and composition control effects.

[0058] The air inlet 342 is flush with the bottom surface of the base plate 320, meaning that steam can directly enter the gas flow pipe 340 as it rises from the distribution pipe body 210 without having to detour or overcome additional structural height differences. This helps reduce gas flow resistance and maintains smooth gas flow. At the same time, the air outlet 341 is located at the end that extends into the extractor 310, allowing the steam to be dispersed and discharged after entering the extractor 310, further promoting heat and mass exchange with the condensed liquid inside the extractor 310.

[0059] This structure not only facilitates uniform introduction of the gas phase and prevents local accumulation of steam, but also improves the uniformity of the gas phase distribution within the extractor 310, making the condensation process more complete. In this way, the light component can smoothly enter the extractor 310 through the gas phase circulation pipe 340, while the heavy component is brought back to the distribution pipe body 210 during contact with the condensed liquid and refluxed to the distillation tower along with the liquid. Therefore, this embodiment achieves smooth conduction of the gas phase path and improved condensation efficiency by optimizing the structure at both ends of the gas phase circulation pipe 340, thereby enhancing the entire system's ability to separate light and heavy components.

[0060] See Figures 1 to 3 In one embodiment, the distance between the overflow port 331 and the substrate 320 is smaller than the distance between the gas outlet 341 and the substrate 320 .

[0061] In this embodiment, the distance between overflow port 331 and substrate 320 is shorter than the distance between gas outlet 341 and substrate 320. That is, overflow port 331 is positioned relatively low, while gas outlet 341 is positioned higher. This structural layout creates a clear liquid-gas stratification control mechanism, further improving the stability and efficiency of gas-liquid separation and interaction.

[0062] Because overflow port 331 is located lower, the condensate in extractor 310 will preferentially reach overflow port 331 as the liquid level gradually rises, and will flow back into distribution pipe 210 through overflow pipe 330. At the same time, vent 341 is located higher, so that the accumulated liquid in extractor 310 will not flood vent 341 during normal operation, thus preventing the gas phase flow pipe 340 from being blocked by liquid or the gas flow path from being interrupted.

[0063] This design ensures that while the reflux liquid is discharged in a timely manner, the steam from the distribution pipe body 210 can still be smoothly introduced into the extractor 310 through the gas phase circulation pipe 340, contacting the condensing surface of the heat exchange component 100, and completing the enrichment process of the light component. At the same time, it also avoids the situation where the light component is "liquid-sealed" or cannot escape in time due to the liquid level being too high. It can be seen that this structure realizes the effective separation and coordinated control of the gas-liquid path in a high-level layout, which helps to further improve the condensation efficiency, separation accuracy, and the stability and reliability of the system operation.

[0064] In one embodiment, the base plate 320 and the sidewall surface of the extractor 310 are integrally formed.

[0065] In this embodiment, the base plate 320 and the sidewall of the extractor 310 are integrally formed. That is, the base plate 320 and the shell of the extractor 310 to which it is connected are integrally formed through an integrated manufacturing process. This structural design has significant advantages in terms of mechanical strength, sealing performance, and simplified manufacturing.

[0066] First, the integrated molding eliminates the potential for joint gaps caused by welding, screwing, or other assembly methods, reducing the risk of liquid or gas leakage at the source and improving the sealing and stability of the extractor 310. Second, the integrated structure eliminates stress concentration at the structural joints, enhancing the entire device's resistance to thermal expansion and contraction, corrosion, and pressure during long-term operation. It is particularly suitable for high-temperature, high-humidity, or corrosive conditions that may exist during the distillation process.

[0067] Furthermore, since the base plate 320 supports key components such as the overflow pipe 330 and the gas-phase flow pipe 340, the integrated molding structure also improves the installation accuracy of internal components, ensures the symmetry of the gas-liquid channel layout and the rationality of the flow path, and promotes uniform distribution and efficient contact between gas and liquid. In summary, this embodiment improves structural strength, sealing reliability, and manufacturing consistency through the integrated molding process, thereby further ensuring the safety, stability, and distillation effect of the entire semiconductor precursor distillation device during use.

[0068] See Figure 2 In one embodiment, a second flange 350 is provided on the outer wall surface of the bottom of the liquid collection component 300, and the second flange 350 protrudes from the outer wall surface of the liquid collection component 300. A third flange 240 is provided on the outer wall surface of the top of the distribution component 200, and the third flange 240 protrudes from the outer wall surface of the distribution component 200. The second flange 350 and the third flange 240 have the same diameter and are matched to connect the liquid collection component 300 and the distribution component 200.

[0069] In this embodiment, a second flange 350 is provided on the outer wall surface of the bottom of the liquid collection component 300, and a third flange 240 is provided on the outer wall surface of the top of the distribution component 200, and both are structures protruding from their respective outer wall surfaces. The second flange 350 and the third flange 240 have the same diameter and are matched and connected, thereby realizing a reliable connection between the liquid collection component 300 and the distribution component 200.

[0070] This flange connection structure offers several technical benefits. First, the provision of equal diameters for the second flange 350 and the third flange 240 facilitates standardized docking between the two components, improving assembly convenience and interchangeability. The flange structure also ensures a high degree of sealing between the two components when connected, effectively preventing gas or condensate leakage and enhancing the safety and stability of device operation.

[0071] Secondly, the protruding flange provides a larger force-bearing area at the connection, thereby enhancing the connection strength. This allows the flange to better withstand internal pressure fluctuations or mechanical vibrations during operation, reducing the risk of failure during device operation. Furthermore, the flange connection facilitates disassembly and maintenance, facilitating the cleaning, replacement, or overhaul of internal structures such as the base plate 320, overflow pipe 330, and gas flow pipe 340, thus facilitating the long-term stable operation and maintenance of the device.

[0072] See Figure 4 In one embodiment, a first temperature control component 400 is further included. The first temperature control component 400 includes a heating pipe 410 arranged in the side wall of the extractor 310. The heating pipe 410 is wound inside the side wall of the extractor 310. The top of the heating pipe 410 is flush with the top of the overflow pipe 330 and is connected to the heat source device for heating the liquid in the extractor 310. The first temperature control component 400 also includes a first temperature sensor for collecting the temperature of the liquid in the extractor 310.

[0073] In this embodiment, the structure further optimizes the gas-liquid contact conditions and separation effect by dynamically controlling the temperature of the condensate in the extractor 310. Specifically, the provision of the heating line 410 can provide heat compensation when the liquid temperature is too low, thereby raising the temperature of the condensate. As a result, when the steam from the distillation tower contacts the reflux condensate in the distribution pipe body 210, the higher liquid temperature effectively reduces the possibility of secondary condensation of the light components during the contact process, preventing them from being carried back to the bottom of the tower, thereby improving the light component removal efficiency during the distillation process.

[0074] Furthermore, the presence of a first temperature sensor enables the system to monitor the temperature of the liquid within extractor 310 in real time and adjust the heating intensity of heating line 410 accordingly, achieving closed-loop control of the liquid temperature. This intelligent temperature control design helps the system maintain optimal gas-liquid equilibrium under various operating conditions, further enhancing the device's ability to effectively separate light and heavy components.

[0075] In one embodiment, a second temperature adjustment component is further included, which is connected to the overflow pipe 330 and is used to heat the liquid in the overflow pipe 330.

[0076] In this embodiment, overflow pipe 330 serves as a crucial channel for condensate to flow back from extractor 310 to distribution pipe 210 and ultimately into the distillation column. The temperature of the liquid within overflow pipe 330 directly affects the mass transfer and heat exchange conditions during contact with steam. By providing a heating function in overflow pipe 330, the second temperature control assembly can prevent premature condensation of light components caused by excessively low liquid temperature, thereby preventing light components from being carried back to the bottom of the distillation column by the liquid. This ensures that light components fully enter extractor 310 before entering heat exchange assembly 100, thereby improving separation efficiency.

[0077] See Figures 2 to 3 In one embodiment, the gas outlet 341 is provided 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.

[0078] In this embodiment, the closed top end face means that after the steam enters the gas phase circulation pipe 340, it cannot be discharged directly in the vertical direction, but must turn to escape from the air outlet 341 on the side wall. The air outlet 341 is set in the area close to the overflow pipe 330, so that the steam is finally discharged from the side wall close to the liquid return path, which is conducive to a more uniform distribution of steam in the extractor 310, while preventing the air flow from directly impacting the top area of ​​the extractor 310, maintaining the stability of the internal gas phase environment. In addition, the top closed structure also has the function of preventing liquid from entering the gas phase circulation pipe 340 from the upper end, further ensuring the purity and smoothness of the gas phase path and preventing cross-contamination between gas and liquid.

[0079] See Figures 1 to 3 In one embodiment, the liquid collecting assembly 300 is provided with a sampling port 360, which is arranged on the side wall surface of the extractor 310 close to the substrate 320. The distance from the sampling port 360 to the substrate 320 is smaller than the distance from the overflow port 331 to the substrate 320. The sampling port 360 is provided with a concentration sensor 370.

[0080] In this embodiment, sampling port 360 is positioned below overflow port 331, enabling sampling to begin before the condensate reaches the overflow level. This allows for earlier and more accurate reflection of the actual concentration trend of the liquid at the bottom of sampler 310. Because the heavy components preferentially condense and collect at the bottom of sampler 310, the liquid sample obtained from sampling port 360 more accurately reflects the proportion of residual light components in the condensate.

[0081] Concentration sensor 370, located at extraction port 360, provides real-time online monitoring of the liquid flowing through it, accurately detecting changes in the concentration of light components in the liquid. When the sensor detects that the concentration reaches a preset threshold, it can be combined with the control system to generate a signal to determine whether the liquid precursor in the distillation column has been completely de-lighted, or to serve as a basis for adjusting the operating status of various system components (such as temperature control, condensation, and reflux).

[0082] An embodiment of the present invention further provides a semiconductor precursor distillation system, including the semiconductor precursor distillation device described above, characterized in that it further includes a distillation tower connected to the distribution component 200 .

[0083] In this embodiment, the distillation tower serves as the initial separation site for the feed gas. A multi-stage mass transfer process within the tower achieves a preliminary separation of the light and heavy components. The separated rising vapor is introduced into the interior of the distribution assembly 200 via a connection structure (such as the connection hole 220 provided on the first flange 230). Within the distribution assembly 200, the vapor further comes into contact with the condensate returning from the liquid collection assembly 300, recaptures and refluxes the heavy components, ensuring they are returned to the distillation tower for secondary distillation. Meanwhile, the light components, uncondensed, continue to rise, ultimately being enriched and discharged.

[0084] The technical features of the above-mentioned embodiments can be combined arbitrarily. In order to make the description concise, not all possible combinations of the technical features in the above-mentioned embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0085] The above-described embodiments merely illustrate several implementations of the present invention, and while their descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the patent. It should be noted that a person skilled in the art would be able to make numerous variations and improvements without departing from the spirit of the present invention, all of which fall within the scope of protection of the present invention. Therefore, the scope of protection of the patent for this invention shall be determined by the appended claims.

Claims

1. A semiconductor precursor distillation device, comprising a heat exchange component (100), characterized in that: Also includes: A distribution assembly (200), the distribution assembly (200) comprising a distribution pipe body (210), the bottom of the distribution pipe body (210) being provided with a connection hole (220) for conveying steam to a distillation tower; A liquid collecting assembly (300) is placed between the distribution pipe body (210) and the heat exchange assembly (100), the liquid collecting assembly (300) comprising a sampler (310) for collecting liquid generated by condensation of the heat exchange assembly (100), a base plate (320) being provided at the bottom of the sampler (310), an overflow pipe (330) and a plurality of gas phase flow pipes (340) being provided on the base plate (320), the gas phase flow pipes (340) being connected between the sampler (310) and the distribution pipe body (210). body (210); one end of the overflow pipe (330) extends into the extractor (310) to form a liquid collecting space (380) with the side wall of the extractor (310); an overflow port (331) is provided on the end of the overflow pipe (330) extending into the extractor (310); the other end extends into the distribution assembly (200) and is located above the connecting hole (220), so that the condensed liquid can contact the steam coming out of the distillation tower in the distribution pipe body (210), thereby flushing the heavy components in the steam; The overflow pipe (330) is located at the center of the base plate (320), a plurality of gas phase flow pipes (340) are arranged around the overflow pipe (330), the overflow pipe (330) and the connecting hole (220) are coaxially arranged, the inner diameter of the overflow pipe (330) is not less than the diameter of the connecting hole (220), and the liquid in the overflow pipe (330) flows back into the distillation tower through the connecting hole (220); An air outlet (341) is provided at one end of the gas phase circulation pipe (340) extending into the extractor (310), and an air inlet (342) is provided at the other end of the gas phase circulation pipe (340). The air inlet (342) is flush with the bottom surface of the substrate (320), and the air outlet (341) is provided on the side wall surface of the overflow pipe (330) away from the substrate (320). The top end surface of the gas phase circulation pipe (340) away from the substrate (320) is closed.

2. The semiconductor precursor distillation device according to claim 1, characterized in that: The overflow port (331) is located at a height exceeding the base plate (320), so that when a certain amount of liquid accumulates in the extractor (310), the liquid enters the overflow pipe (330) through the overflow port (331).

3. The semiconductor precursor distillation device according to claim 1, wherein: A first flange (230) for connecting to a distillation tower is provided at the bottom of the distribution pipe body (210), and the connecting hole (220) is provided on the first flange (230).

4. The semiconductor precursor distillation device according to claim 1, wherein: The distance between the overflow port (331) and the substrate (320) is smaller than the distance between the air outlet (341) and the substrate (320).

5. The semiconductor precursor distillation device according to claim 1, wherein: The base plate (320) and the side wall surface of the extractor (310) are integrally formed.

6. The semiconductor precursor distillation device according to claim 1, characterized in that: A second flange (350) is provided on the outer wall surface of the bottom of the liquid collecting component (300), and the second flange (350) protrudes from the outer wall surface of the liquid collecting component (300). A third flange (240) is provided on the outer wall surface of the top of the distribution component (200), and the third flange (240) protrudes from the outer wall surface of the distribution component (200). The second flange (350) and the third flange (240) have the same diameter and are matched to connect the liquid collecting component (300) and the distribution component (200).

7. The semiconductor precursor distillation device according to claim 1, wherein: The invention also includes a first temperature control component (400), which includes a heating pipeline (410) arranged in the side wall of the extractor (310). The heating pipeline (410) is arranged around 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 in the extractor (310). The first temperature control component (400) also includes a first temperature sensor for collecting the temperature of the liquid in the extractor (310).

8. The semiconductor precursor distillation device according to claim 1, wherein: It also includes a second temperature adjustment component, which is connected to the overflow pipe (330) and is used to heat the liquid in the overflow pipe (330).

9. The semiconductor precursor distillation device according to claim 1, wherein: The liquid collecting component (300) is provided with a sampling port (360), and the sampling port (360) is arranged on a side wall surface of the extractor (310) close to the substrate (320). The distance between the sampling port (360) and the substrate (320) is smaller than the distance between the overflow port (331) and the substrate (320). The sampling port (360) is provided with a concentration sensor (370).

10. A semiconductor precursor distillation system, comprising the semiconductor precursor distillation device according to any one of claims 1 to 9, characterized in that: Also included is a distillation tower connected to the distribution assembly (200).

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