CN120242518A - A semiconductor precursor distillation device, system and method - Google Patents

Abstract

The invention discloses a semiconductor precursor distillation device, system and method, comprising a heat exchange component, a distribution component and a liquid collecting component, wherein the distribution component comprises a distribution pipe body, and a connection hole for conveying steam to a distillation tower is provided at the bottom of the distribution pipe body; the liquid collecting component is placed between the distribution pipe body and the heat exchange component, and comprises an extractor for collecting liquid generated by condensation of the heat exchange component, and a base plate is provided at the bottom of the extractor, and 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, so as to flush 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 the light component substances in the semiconductor precursor is reduced.

Description

Precursor rectifying device, system and method for semiconductor

Technical Field

The invention relates to the technical field of semiconductor materials, in particular to a precursor rectifying device, a precursor rectifying system and a precursor rectifying method for a semiconductor.

Background

As semiconductor fabrication processes advance to technology nodes of 5 nm and below, the preparation of high purity semiconductor precursors (e.g., metal-organic, halides, etc.) becomes a critical challenge. The purity of the semiconductor precursor directly affects the performance and reliability of the chip, and particularly, the residues of metal impurities, oxygen-containing pollutants and particulate matters need to be controlled at ppb (parts per billion) level, which puts near-limiting demands on the traditional chemical rectification technology. However, the purification scene of the semiconductor precursor has a significant difference from the traditional chemical industry field that the former needs to realize impurity separation under the conditions of small batch and high precision, the latter usually takes large-scale continuous production as a core target, the traditional chemical industry rectification usually processes ton-level materials and allows larger component fluctuation, the precursor rectification needs to realize ppb-level impurity control under the kilogram-level operation amount, and the two are difficult to be compatible in process design logic.

Patent CN201384866Y provides a vertical automatic reflux extraction rectification device. The device consists of a mist catcher, a tube condenser, a reflux extraction controller, an overhead extraction port, a rectifying tower, an extraction flowmeter, an extraction regulating valve and a tower kettle reboiler. The material is evaporated by a tower kettle reboiler, heat and mass transfer are carried out in the tower, the material steam enters a tower top tubular condenser to be condensed and descends into a liquid collecting tank of a reflux extraction controller, condensed liquid enters an annular liquid collecting cavity from two ends of the liquid collecting tank, part of the condensed liquid is guided by a guide cylinder through overflow holes on the side surface of an overflow weir to be redistributed and refluxed, the part of the condensed liquid is distributed through a tear hole, part of the condensed liquid is extracted from a tower top extraction port through a flowmeter and a regulating valve, and non-condensable gas is pumped out from a tower top vacuum port after liquid drops are removed through a mist trap.

However, while the upright auto reflux extraction rectification apparatus provided by the above-mentioned patent is widely used in the traditional chemical industry, it exposes a series of limitations in the purification of semiconductor precursors. Firstly, the theoretical plate number and the separation efficiency of the traditional device are difficult to meet the separation requirement of light and heavy components with similar boiling points, so that the impurity residue is far higher than the requirement of a semiconductor process, and the separation efficiency is difficult to improve.

Disclosure of Invention

Accordingly, it is desirable to provide a precursor rectification apparatus, system, and method for semiconductors that address the above-described problem of insufficient gas-liquid phase separation.

The application provides a precursor rectifying device for a semiconductor, which comprises a heat exchange assembly and further comprises:

The distribution assembly comprises a distribution pipe body, and a connecting hole for the rectifying tower to convey steam is formed in the bottom of the distribution pipe body;

The liquid collecting assembly is arranged between the distribution pipe body and the heat exchange assembly, the liquid collecting assembly comprises a collector for collecting liquid generated by condensation of the heat exchange assembly, a base plate is arranged at the bottom of the collector, an overflow pipe and a plurality of gas-phase flow pipes are arranged on the base plate, the gas-phase flow pipes are communicated with the collector and the distribution pipe body, one end of the overflow pipe extends into the collector to form a liquid collecting space with the side wall surface of the collector, an overflow port is arranged at one end of the overflow pipe extending into the collector, the other end of the overflow pipe extends into the distribution assembly and is positioned above the connecting hole, so that condensate can be contacted with steam coming out of the rectifying tower in the distribution pipe body, and heavy component substances in the flushing steam are realized.

Optionally, the overflow pipe is located at a central position of the base plate, and a plurality of gas phase flow pipes are arranged around the overflow pipe.

Optionally, the overflow port is located at a height above the base plate such that liquid within the extractor accumulates a certain amount and enters the overflow tube through the overflow port.

Optionally, the overflow pipe and the connecting hole are coaxially arranged, the inner diameter of the overflow pipe is not smaller than the diameter of the connecting hole, and the liquid in the overflow pipe flows back into the rectifying tower through the connecting hole.

Optionally, a first flange for connecting the rectifying tower is arranged at the bottom of the distribution pipe body, and the connecting hole is formed in the first flange.

Optionally, an air outlet hole is formed at one end of the gas phase flow pipe extending into the extractor, an air inlet hole is formed at the other end of the gas phase flow pipe, and the air inlet hole is flush with the bottom surface of the base plate.

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

Optionally, the substrate and the sidewall surface of the extractor are integrally formed.

Optionally, be equipped with the second flange on the lateral wall of collection liquid subassembly bottom, the second flange protrusion collection liquid subassembly's lateral wall sets up, be equipped with the third flange on the lateral wall at distribution subassembly top, the third flange protrusion distribution subassembly's lateral wall sets up, the second flange is connected with the cooperation with the third flange constant diameter, in order to connect collection liquid subassembly and distribution subassembly.

Optionally, the device further comprises a first temperature adjusting component, the first temperature adjusting component comprises 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 connected with a heat source device for heating liquid in the extractor, and the first temperature adjusting component further comprises a first temperature sensor for collecting the temperature of the liquid in the extractor.

Optionally, a second temperature regulating assembly is further included, and the second temperature regulating assembly is connected with the overflow pipe and is used for heating the liquid in the overflow pipe.

Optionally, the air outlet hole is arranged on a side wall surface of one side, far away from the base plate, of the overflow pipe, and the top end surface of one side, far away from the base plate, of the gas-phase flow pipe is arranged in a closed manner.

Optionally, the liquid collecting component is provided with a collecting outlet, the collecting outlet is arranged on a side wall surface, close to the substrate, in the collecting device, the distance from the collecting outlet to the substrate is smaller than the distance from the overflow port to the substrate, and the collecting outlet is provided with a concentration sensor.

The application also provides a precursor rectifying system for the semiconductor, which comprises the precursor rectifying device for the semiconductor and further comprises a rectifying tower, wherein the rectifying tower is connected with the distribution assembly.

The application also provides a precursor rectifying method for the semiconductor, which adopts the precursor rectifying system for the semiconductor and comprises the following steps:

And adjusting the temperature of the rectifying tower to be the evaporation temperature T1, wherein the 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 in the rectifying tower.

And adjusting the heat exchange assembly to a condensation temperature T2, wherein T2 is smaller than Tb, and collecting liquid generated by condensation of the heat exchange assembly until the liquid is collected in the extraction cavity and flows into the overflow pipe.

And adjusting the first temperature adjusting assembly until the temperature of the liquid in the extraction cavity reaches T3, wherein T3 is the Tb floating coefficient K1.

And adjusting the second temperature adjusting component until the temperature of the liquid in the overflow pipe reaches T4, wherein T4 is the Tb floating coefficient K2.

And (3) continuing evaporating until the concentration of the light component B in the liquid in the extraction cavity reaches a threshold value, and judging that the liquid precursor in the rectifying tower is subjected to light removal.

Compared with the prior art, the technical scheme provided by the application has the following beneficial effects:

The connecting holes at the bottom of the distributing pipe body are communicated with the steam outlets of the rectifying tower, so that rising steam is diffused along the inner space of the distributing pipe body, and the extractor of the liquid collecting component is connected with the distributing pipe body through a gas phase runner pipe on the base plate in a gas path. The steam vertically enters the top space of the extractor through the gas-phase flow pipe upwards and is further conveyed to the heat exchange assembly for condensation. In the process, the condensed liquid collected in the extractor flows reversely through the overflow pipe below the base plate, one end of the overflow pipe extends into the distribution pipe body, and the overflow port of the overflow pipe is higher than the position of the connecting hole, so that the reflux liquid forms countercurrent contact with new rising steam entering from the connecting hole when flowing from top to bottom in the distribution pipe body. The condensed liquid has scouring action on heavy component liquid drops or high boiling point substances which are carried in the steam and are not completely vaporized, so that heavy components are forced to flow back to the rectifying tower along with the liquid to participate in rectification again, and light components in the steam enter the heat exchange component through the gas phase flow pipe due to boiling point difference. The even arrangement of the gas-phase flow pipes on the base plate not only ensures the even distribution of the steam flow, but also prevents the liquid from flowing backward to the distribution pipe body when the steam pressure fluctuates through the physical blocking effect of the base plate on the liquid in the extractor. Meanwhile, the height of the overflow port limits the upper limit of the liquid level in the extractor, and when the volume of the condensate exceeds the height of the overflow port, excessive liquid is automatically discharged through the overflow pipe, so that the dynamic update of the light component condensate in the extractor is maintained, and the gas phase flow pipe is prevented from being blocked by the liquid due to the overhigh liquid level. The heat exchange assembly continuously condenses light component steam and collects and discharges the extractor to form a closed loop, so that light component substances are continuously concentrated and discharged out of the system, heavy components are trapped and returned to the rectifying tower through gas-liquid countercurrent contact, enrichment of the heavy components at the top of the rectifying tower is reduced, high-efficiency removal of light component impurities in the semiconductor precursor and circulating purification of the heavy components are finally realized, and separation efficiency is improved.

Drawings

FIG. 1 is a schematic cross-sectional view of a precursor rectifying apparatus for semiconductor according to an embodiment of the present application;

FIG. 2 is a schematic cross-sectional view of a liquid collecting module and a distributing module of a precursor rectifying apparatus for semiconductor according to an embodiment of the present application;

FIG. 3 is a schematic view of a liquid collecting assembly of a precursor rectifying apparatus for semiconductor according to an embodiment of the present application;

FIG. 4 is a schematic diagram of a first temperature adjusting component of a precursor rectification apparatus for semiconductor according to an embodiment of the present application;

fig. 5 is an external configuration diagram of a precursor rectification apparatus for semiconductor according to an embodiment of the present application.

Reference numerals illustrate:

100. The heat exchange device comprises a heat exchange assembly, a distribution assembly, a 210, a distribution pipe body, a 220, a connecting hole, a 230, a first flange, a 240, a third flange, a 300, a liquid collecting assembly, a 310, a extractor, a 320, a base plate, a 330, an overflow pipe, a 331, an overflow port, a 340, a gas phase runner pipe, a 341, an air outlet hole, a 342, an air inlet hole, a 350, a second flange, a 360, a extraction port, a 370, a concentration sensor, a 380, a liquid collecting space, a 400, a first temperature adjusting assembly, a 410 and a heating pipeline.

Detailed Description

In order that the above objects, features and advantages of the invention will be readily understood, a more particular description of the invention will be rendered by reference to the appended drawings. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. The present invention may be embodied in many other forms than described herein and similarly modified by those skilled in the art without departing from the spirit of the invention, whereby the invention is not limited to the specific embodiments disclosed below.

In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings are merely for convenience in describing the present invention and simplifying the description, and do not indicate or imply that the device or element being referred to must have a specific orientation, be configured and operated in a specific orientation, and therefore should not be construed as limiting the present invention.

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

In the present invention, unless explicitly specified and limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally formed, mechanically connected, electrically connected, directly connected, indirectly connected through an intervening medium, or in communication between two elements or in an interaction relationship between two elements, unless otherwise explicitly specified. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.

Referring to fig. 1 to 3, an embodiment of the present invention provides a precursor rectification apparatus for a semiconductor, including a heat exchange assembly 100, further including:

the distribution assembly 200, the distribution assembly 200 comprises a distribution pipe body 210, and a connecting hole 220 for the rectifying tower to convey steam is arranged at the bottom of the distribution pipe body 210;

The liquid collecting assembly 300 is arranged between the distribution pipe body 210 and the heat exchange assembly 100, the liquid collecting assembly 300 comprises a collector 310 for collecting liquid generated by condensation of the heat exchange assembly 100, a base plate 320 is arranged at the bottom of the collector 310, an overflow pipe 330 and a plurality of gas-phase flow pipes 340 are arranged on the base plate 320, the gas-phase flow pipes 340 are communicated with the collector 310 and the distribution pipe body 210, one end of the overflow pipe 330 extends into the collector 310 to form a liquid collecting space 380 with the side wall surface of the collector 310, one end of the overflow pipe 330 extends into the collector 310, an overflow port 331 is arranged at the other end of the overflow pipe 330 extends into the distribution assembly 200 and is positioned above the connecting hole 220, so that condensate can be contacted with steam from the rectifying tower in the distribution pipe body 210 to flush heavy component substances in the steam, then flows back into the rectifying tower together, corresponding light component substances can be enriched rapidly, and the light component substances can be discharged timely, and the light component substances in the semiconductor precursor can be reduced.

Referring to fig. 2, the descending arrow in the figure is the liquid generated by condensation, the ascending arrow is the vapor generated by the rectifying tower, and the dotted line square area is the area where the condensed liquid contacts with the vapor and generates a flushing effect.

In this embodiment, the connection hole 220 at the bottom of the distribution pipe 210 is communicated with the steam outlet of the rectifying tower, so that the rising steam diffuses along the inner space of the distribution pipe 210, and the extractor 310 of the liquid collecting assembly 300 is connected with the distribution pipe 210 through the gas phase flow pipe 340 on the base plate 320 in a gas path. The vapor passes vertically upward through the vapor flow tube 340 into the head space of the extractor 310 and is further conveyed to the heat exchange assembly 100 for condensation. In this process, the condensed liquid collected in the extractor 310 flows reversely through the overflow pipe 330 under the base plate 320, and one end of the overflow pipe 330 extends into the distribution pipe 210 and the overflow port 331 thereof is higher than the position of the connection hole 220, so that the reflux liquid forms countercurrent contact with the newly rising steam entering from the connection hole 220 when flowing from top to bottom in the distribution pipe 210. The condensate has a scouring action on the droplets of heavy components or high boiling point substances which are not completely vaporized and are entrained in the steam, the heavy components are forced to flow back to the rectifying tower along with the liquid to participate in rectification again, and the light components in the steam enter the heat exchange component 100 through the gas phase flow pipe 340 due to the difference of boiling points. The uniform arrangement of the gas-phase flow tubes 340 on the base plate 320 not only ensures uniform distribution of the vapor flow rate, but also prevents the liquid from flowing backward to the distribution tube body 210 when the vapor pressure fluctuates by the physical barrier effect of the base plate 320 on the liquid in the extractor 310. Meanwhile, the height of the overflow port 331 defines 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 excessive liquid is automatically discharged through the overflow pipe 330, so that the dynamic update of the light component condensate in the extractor 310 is maintained, and the gas phase flow tube 340 is prevented from being blocked by the liquid due to the overhigh 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 out of the system, while the heavy component is trapped and returned to the rectifying tower through the countercurrent contact of the gas and the liquid, thereby reducing the enrichment of the heavy component at the top of the rectifying tower, finally realizing the efficient removal of the light component impurities in the semiconductor precursor and the cyclic purification of the heavy component, and improving the separation efficiency.

In the prior art, condensate generated by the shell-and-tube condenser needs to be refluxed and extracted through a guide cylinder, an overflow weir, a tear hole and other multi-stage distribution structures, and the separation efficiency is limited by a static overflow mechanism and a passive flow guiding mechanism. For example, the overflow holes on the side of the overflow weir can only control the reflux amount through the fixed aperture, and the capillary action of the tear holes can assist the liquid distribution, but the extraction proportion of the light components is difficult to accurately adjust, and particularly when a light and heavy component system with close boiling points and fine physical property differences is treated, secondary entrainment of condensate or light component residue is easy to cause. In addition, although the mist trap can intercept liquid drops in the gas phase, active interception of heavy component molecules which are not completely condensed in steam cannot be realized, and finally the light component content is difficult to break through a threshold value of 2%.

Further, the cooperative design of the gas-phase flow tube 340 and the substrate 320 overcomes the defect of cross interference of gas-liquid paths in the conventional apparatus. The uniform arrangement of the gas-phase flow pipes 340 on the substrate 320 not only realizes the homogenization and distribution of the steam flow, but also completely isolates the rising steam from the falling liquid through the physical barrier of the substrate 320, thereby fundamentally eliminating the reduction of mass transfer efficiency caused by the mixing of gas-liquid two-phase flow in the prior art. For example, although the structure of the guide cylinder and the tear holes in CN201384866Y can guide the liquid distribution, it is unavoidable that the rising vapor and the reflux liquid are partially mixed in the liquid collecting tank, so that part of the light components are wrapped and entrained in the reflux liquid and returned to the tower, and in this embodiment, the space isolation of the base plate 320 and the directional diversion of the gas phase runner 340 ensure that the light component vapor directly reaches the condensation area under the condition of no interference, so as to realize the rapid enrichment and directional discharge of the light components.

Referring to fig. 1 to 3, in one embodiment, the overflow pipe 330 is positioned at a central position of the base plate 320, and a plurality of gas phase flow pipes 340 are disposed around the overflow pipe 330.

In this embodiment, the overflow pipe 330 is located at the center of the base plate 320, and a plurality of gas phase flow pipes 340 are disposed around the overflow pipe 330. This structural arrangement further optimizes the contact path and contact efficiency of the liquid with the gas within the distribution pipe body 210. Specifically, the overflow pipe 330 at the center position can make the condensed liquid collected in the extractor 310 flow back into the distribution pipe body 210 preferentially from the center region, and the vapor from the distribution pipe body 210 uniformly rises to the base plate 320 from the periphery and enters the extractor 310 through the vapor flow pipe 340 in the process of flowing to the extractor 310 due to the structure surrounded by the vapor flow pipe 340 arranged around the central region.

The arrangement of the gas phase and the liquid phase which are uniformly distributed from the center to the outside ensures that the gas phase and the liquid phase are in more sufficient and uniform contact in the distribution pipe body 210, and improves the scouring effect of condensate on heavy component substances in steam. Meanwhile, the layout is favorable for maintaining the stability of gas-liquid flow in the device, and local turbulence or bias current is avoided, so that the efficiency of the rectification process is further improved. Therefore, the structure can more effectively realize the recovery of the heavy component and the enrichment of the light component, is beneficial to reducing the content of the light component substances in the final product and improves the purity of the semiconductor precursor.

Referring to fig. 1-3, in one embodiment, overflow port 331 is positioned at a height above substrate 320 such that liquid within extractor 310 accumulates a certain amount and enters overflow tube 330 through overflow port 331.

In this embodiment, the overflow port 331 is located at a height higher than the base plate 320, so that condensate in the extractor 310 can enter the overflow pipe 330 through the overflow port 331 and flow back to the distribution pipe 210 after accumulating to a certain level. By providing the overflow port 331 at a position higher than the base plate 320, a liquid level control structure is formed to ensure that condensate does not immediately flow into the distribution pipe body 210, but remains in the extractor 310 for a certain period of time, and is accumulated to a set height before being discharged through the overflow port 331.

The structure has the technical effect that the flow rate and the flow velocity of the reflux liquid can be effectively controlled, 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 remaining light components in the extractor 310, but also prevents the disturbance of the gas-liquid contact state in the lower distribution pipe body 210 by condensate fluctuation. Meanwhile, the liquid can flow back only after the liquid level reaches the height of the overflow port 331, so that the liquid can be prevented from flowing back in a direct short circuit, and the operation controllability of the device and the stability of rectification separation are enhanced. Therefore, by controlling the overflow liquid level, the embodiment realizes more efficient and controllable condensate reflux and is beneficial to improving the separation precision of the light and heavy components in the precursor.

Referring to fig. 1 to 3, in one embodiment, the overflow pipe 330 is coaxially disposed with the connection hole 220, the inner diameter of the overflow pipe 330 is not smaller 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.

In this embodiment, the overflow pipe 330 is coaxially disposed with the connection hole 220, and the inner diameter of the overflow pipe 330 is not smaller than the diameter of the connection hole 220, so that the liquid in the overflow pipe 330 can smoothly flow back into the rectifying tower through the connection hole 220. The structure design has a definite flow guiding function, can realize the linearization and centering of a backflow path through coaxial arrangement, and is beneficial to improving the stability and efficiency of liquid backflow.

Because the liquid in the overflow pipe 330 directly flows back to the rectifying tower through the connecting hole 220, the liquid accumulation or flow resistance possibly caused by the middle redundant flow channel or turning is avoided, thereby 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 smaller than the diameter of the connecting hole 220, so that the full coverage of the connecting hole 220 is realized, and the flushing effect is improved.

Through the structural arrangement, the condensate can be efficiently and smoothly refluxed, heavy components carried in the steam can be brought back to the rectifying tower in time to be separated again, so that the separation precision is improved, the composition of substances in the tower is stabilized, and the technical effects of reducing the content of light components in the precursor and improving the purity of the product are finally achieved.

Referring to fig. 2, in one embodiment, a first flange 230 for connecting to the rectifying tower is provided at the bottom of the distribution pipe body 210, and the connection hole 220 is provided on the first flange 230.

In this embodiment, a first flange 230 for connecting to the rectifying tower is disposed at the bottom of the distribution pipe 210, and the connection hole 220 is disposed on the first flange 230. By integrating the connection hole 220 at the position of the first flange 230, not only is a compact integration achieved in structure, but also the installation butt joint and sealing performance of the device are improved.

The first flange 230 serves as a connection interface between the distribution pipe body 210 and the rectifying tower, and is provided such that the entire distribution assembly 200 can be conveniently docked with the rectifying tower through a standard flange structure, simplifying an assembly process, and enhancing structural stability and maintainability. The connection holes 220 are located on the first flange 230, so that the steam from the rectifying tower can directly enter the inside of the distributing pipe body 210 from bottom to top, thereby realizing direct contact and exchange between the steam and condensate.

The design not only improves the sealing reliability of the connecting part and avoids steam leakage, but also ensures that the structural relationship between the steam channel and the liquid reflux path is more definite and the flow is smoother, thereby being beneficial to maintaining the stability of the system operation and the continuity of the separation process. Therefore, the embodiment further optimizes the vapor transmission and liquid reflux path while ensuring stable connection of the device through the integrated design of the flange structure and the connecting hole 220, thereby helping to improve the overall rectification efficiency and the product quality.

Referring to fig. 2 to 3, in one embodiment, an air outlet 341 is formed at an end of the gas phase flow tube 340 extending into the extractor 310, an air inlet 342 is formed at the other end of the gas phase flow tube 340, and the air inlet 342 is flush with the bottom surface of the base plate 320.

In this embodiment, an air outlet 341 is formed at one end of the gas-phase flow tube 340 extending into the extractor 310 for guiding the gas-phase material from the distribution tube 210 into the extractor 310, and an air inlet 342 is formed at the other end of the gas-phase flow tube 340, and the air inlet 342 is flush with the bottom surface of the base plate 320. The structural design optimizes the flow path and the transmission efficiency of the gas phase, thereby further improving the effects of gas-liquid separation and component control.

The air inlet 342 is flush with the bottom surface of the base plate 320, which means that the steam can directly enter the gas phase flow tube 340 during the process of rising from the inside of the distribution pipe body 210, without bypassing or overcoming the additional structural height difference, which is beneficial to reducing the gas flow resistance and keeping the gas phase flow stable. Meanwhile, the air outlet hole 341 is disposed at one end extending into the inside of the extractor 310, so that the steam can be dispersed and discharged after entering the extractor 310, thereby further promoting the heat and mass exchange with the condensed liquid inside the extractor 310.

This structure not only helps to uniformly introduce the gas phase and prevent partial accumulation of the vapor, but also improves the uniformity of the gas phase distribution inside the extractor 310, making the condensation process more complete. In this way, the light fraction may smoothly enter the extractor 310 through the gas phase flow pipe 340, while the heavy fraction is brought back to the distribution pipe 210 during contact with the condensed liquid and flows back to the rectifying column with the liquid. Therefore, the embodiment realizes smooth conduction of the gas phase path and improvement of condensation efficiency through optimization of the structures at the two ends of the gas phase flow pipe 340, thereby enhancing the separation capability of the whole system on light and heavy components.

Referring to fig. 1-3, in one embodiment, the overflow port 331 is less distant from the substrate 320 than the gas outlet hole 341 is distant from the substrate 320.

In this embodiment, the distance from the overflow port 331 to the substrate 320 is smaller than the distance from the outlet hole 341 to the substrate 320, i.e. the position of the overflow port 331 is relatively lower, and the outlet hole 341 is located higher. The structure layout forms a clear liquid-gas layering control mechanism, and further improves the stability and efficiency of gas-liquid separation and interaction.

Because the overflow port 331 is lower, condensate in the extractor 310 will preferentially reach the overflow port 331 and flow back to the distribution pipe 210 through the overflow pipe 330 during the gradual rise of the liquid level. Meanwhile, the position of the air outlet hole 341 is higher, so that the accumulated liquid in the extractor 310 will not submerge the air outlet hole 341 in the normal working state, thereby avoiding the problem that the gas phase flow tube 340 is blocked by the liquid or the gas flow path is blocked.

This design ensures that the vapor from the distribution pipe 210 can still be smoothly introduced into the extractor 310 through the vapor phase flow pipe 340 while the reflux liquid is timely discharged, and contacts the condensation surface of the heat exchange assembly 100, thereby completing the enrichment process of the light components. Meanwhile, the situation that light components are sealed by liquid or cannot escape in time due to the fact that the liquid level is too high is avoided. Therefore, the structure realizes effective separation and cooperative control of the gas-liquid paths on the height layout, thereby being beneficial to further improving the condensation efficiency, the separation precision and the stability and the reliability of the system operation.

In one embodiment, the base 320 is integrally formed with the sidewall surface of the extractor 310.

In this embodiment, the base plate 320 and the sidewall surface of the extractor 310 are integrally formed, i.e. the casing of the extractor 310 to which the base plate 320 is connected is integrally formed by an integral manufacturing process. The structural design has remarkable advantages in mechanical strength, sealing performance, manufacturing simplification and the like.

First, the integral formation avoids connection gaps that may be caused by welding, screwing or other assembly methods, reduces the risk of liquid or gas leakage from the source, and improves the tightness and stability of the inside of the extractor 310. And secondly, the integral structure eliminates the problem of stress concentration at the structural joint, enhances the capability of heat expansion and cold contraction resistance, corrosion resistance and pressure resistance of the whole device in long-term operation, and is particularly suitable for high-temperature, high-humidity or corrosion working conditions possibly existing in the rectification process.

In addition, since the substrate 320 plays a role of supporting key components such as the overflow pipe 330 and the vapor phase flow pipe 340, the integrated molding structure can also improve the installation precision of internal components, ensure the symmetry of the arrangement of the vapor-liquid channels and the rationality of the flow paths, and facilitate the uniform distribution and efficient contact of the vapor and the liquid. In conclusion, the embodiment improves the structural strength, the sealing reliability and the manufacturing consistency through the integrated forming process, so that the safety, the stability and the rectifying effect of the whole set of semiconductor precursor rectifying device in the use process are further ensured.

Referring to fig. 2, in one embodiment, a second flange 350 is disposed on an outer side wall surface of 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 disposed on an 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 equal in diameter and are cooperatively connected to each other to connect the liquid collecting assembly 300 and the distribution assembly 200.

In this embodiment, the outer side wall surface of the bottom of the liquid collecting assembly 300 is provided with the second flange 350, the outer side wall surface of the top of the distribution assembly 200 is provided with the third flange 240, and both are structures protruding from the respective outer side wall surfaces, and the diameters of the second flange 350 and the third flange 240 are the same and are in fit connection, so that reliable connection between the liquid collecting assembly 300 and the distribution assembly 200 is realized.

The flange connection structure has various technical effects. Firstly, by arranging the second flange 350 and the third flange 240 with equal diameters, standardized butt joint between the two components is facilitated, and convenience and interchangeability of assembly are improved. The flange structure is adopted to ensure that the two components can realize higher sealing performance when being connected, so that leakage of gas or condensate is effectively prevented, and the operation safety and stability of the device are improved.

Secondly, the protruding setting of flange makes the junction portion possess bigger area of force to reinforcing joint strength can bear inside pressure fluctuation or mechanical vibration better in actual operation, reduces the trouble risk in the device use. In addition, the flange connection mode is convenient to detach and maintain, and is convenient to clean, replace or overhaul the internal structures such as the base plate 320, the overflow pipe 330, the gas-phase runner pipe 340 and the like, so that the long-term stable operation and maintenance management of the device are facilitated.

Referring to fig. 4, in one embodiment, the first temperature adjusting assembly 400 further includes a heating pipe 410 disposed in a sidewall of the extractor 310, the heating pipe 410 is wound around the sidewall of the extractor 310, a top of the heating pipe 410 is flush with a top of the overflow pipe 330 and is connected with a heat source device for heating the liquid in the extractor 310, and the first temperature adjusting assembly 400 further includes a first temperature sensor for collecting a temperature of the liquid in the extractor 310.

In this embodiment, the structure further optimizes the gas-liquid contact condition and separation effect by dynamically controlling the temperature of the condensate in the extractor 310. Specifically, the heating circuit 410 is configured to provide thermal compensation when the liquid temperature is too low, raising the temperature of the condensate. In this way, when the vapor from the rectifying tower contacts with the reflux condensate in the distributing pipe 210, the possibility of secondary condensation of the light component in the contacting process can be effectively reduced due to the higher liquid temperature, and the light component is prevented from being brought back to the bottom of the tower, so that the light component removing efficiency in the rectifying process is improved.

In addition, the first temperature sensor is configured to enable the system to monitor the temperature state of the liquid in the extractor 310 in real time, and adjust the heating intensity of the heating pipeline 410 accordingly, so as to realize closed-loop control over the liquid temperature. The intelligent temperature adjustment design is beneficial to maintaining the optimal gas-liquid balance state of the system under different working conditions, and further enhances the effective separation of the device on the light and heavy components.

In one embodiment, a second temperature regulating assembly is also included, coupled to overflow tube 330, for heating the liquid within overflow tube 330.

In this embodiment, the overflow pipe 330 is an important passage for condensate to flow back from the extractor 310 to the distribution pipe 210 and finally to the rectifying tower, and the temperature of the liquid inside will directly affect the mass transfer and heat exchange state when contacting with steam. Through setting up the heating function at overflow pipe 330, the light component that the second temperature regulating assembly can prevent that liquid temperature from excessively low from causing condenses in advance to avoid light component to be brought back to rectifying column bottom by liquid, ensure that light component gets into heat exchange assembly 100 after fully getting into extractor 310, promote separation efficiency.

Referring to fig. 2 to 3, in one embodiment, the gas outlet hole 341 is disposed on a side wall surface of the overflow pipe 330 on a side away from the base plate 320, and the top end surface of the gas phase flow pipe 340 on a side away from the base plate 320 is disposed in a closed manner.

In this embodiment, the closed top end surface means that the steam, after entering the gas phase flow tube 340, cannot be directly discharged in the vertical direction, but must be diverted to escape from the gas outlet hole 341 in the side wall. The gas outlet 341 is disposed in the area near the overflow pipe 330, so that the steam is finally discharged from the side wall near the liquid return path, which is favorable for more uniformly distributing the steam in the extractor 310, and simultaneously, the gas flow is prevented from directly impacting the top area of the extractor 310, so that the stability of the internal gas phase environment is maintained. In addition, the top sealing structure also has the function of preventing liquid from entering the gas-phase flow pipe 340 from the upper end, further guaranteeing the purity and smoothness of the gas-phase path and preventing gas-liquid cross contamination.

Referring to fig. 1 to 3, in one embodiment, the liquid collecting assembly 300 is provided with a collecting outlet 360, the collecting outlet 360 is disposed on a side wall surface of the collector 310 near the substrate 320, a distance from the collecting outlet 360 to the substrate 320 is smaller than a distance from the overflow port 331 to the substrate 320, and a concentration sensor 370 is disposed on the collecting outlet 360.

In this embodiment, the outlet 360 is disposed below the overflow port 331, so that it can start sampling when the condensate has not reached the overflow level, so as to reflect the actual concentration trend of the liquid at the bottom of the extractor 310 earlier and more accurately. Because the heavy components preferentially condense and pool at the bottom of the extractor 310, the liquid sample obtained at the extraction port 360 can more truly represent the proportion of the residual light components in the condensate.

The concentration sensor 370 is disposed on the outlet 360, and can perform real-time on-line monitoring on the liquid flowing through the position, and accurately detect the concentration change of the light component in the liquid. When the sensor detects that the concentration reaches a preset threshold value, a signal can be sent by combining with the control system to judge whether the liquid precursor in the rectifying tower is completely light or not, or the signal can be used as a basis for regulating the running states (such as temperature adjustment, condensation, reflux and the like) of all parts of the system.

The embodiment of the invention also provides a precursor rectification system for the semiconductor, which comprises the precursor rectification device for the semiconductor and is characterized by further comprising a rectification tower, wherein the rectification tower is connected with the distribution assembly 200.

In this embodiment, the rectifying tower is used as a primary separation site for the raw gas, and the light and heavy components are primarily separated through a multistage mass transfer process in the rectifying tower, and the separated rising steam is introduced into the distribution assembly 200 through a connection structure (such as a connection hole 220 provided on the first flange 230). In the distribution assembly 200, the steam further contacts with condensate flowing back from the liquid collecting assembly 300 to capture and flow back again heavy components, so that the heavy components are guaranteed to be brought back into the rectifying tower for secondary rectification, and meanwhile, light components continue to rise due to non-condensation, so that final enrichment and discharge are achieved.

The embodiment of the invention also provides a precursor rectifying method for the semiconductor, which adopts the precursor rectifying system for the semiconductor, and is characterized by comprising the following steps of:

the temperature of the rectifying tower is regulated to be the evaporating temperature T1, and the 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 in the rectifying tower.

The heat exchange assembly 100 is adjusted to a condensation temperature T2, T2 less than Tb, and the liquid resulting from condensation of the heat exchange assembly 100 is collected until the liquid collects in the extractor 310 and flows into the overflow tube 330.

The first temperature adjustment assembly 400 is adjusted until the temperature of the liquid in the extractor 310 reaches T3, where T3 is tb×floating coefficient K1.

The second temperature adjusting component is adjusted until the temperature of the liquid in the overflow pipe 330 reaches T4, and T4 is Tb, the floating coefficient K2.

And continuing to evaporate until the concentration of the light component B in the liquid in the extractor 310 reaches a threshold value, and judging that the liquid precursor in the rectifying tower is completely light.

In this embodiment, first, by heating the rectifying column, the temperature in the column is adjusted to the evaporation temperature T1, the temperature T1 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 is kept in a liquid state, and the light component B is converted into steam to enter the upper space, thereby forming preliminary separation of the light and heavy components.

Subsequently, the heat exchange assembly 100 is adjusted to a condensing temperature T2, T2 below the boiling point Tb of the light fraction B, such that a portion of the vapor condenses on the surface of the heat exchange assembly 100, and the condensed liquid, after pooling, flows into the extractor 310 and is brought back through the overflow pipe 330. The condensate serving as a flushing fluid can effectively adsorb and carry heavy components entrained in the steam in the process of contacting the condensate with the steam from the rectifying tower, so that the heavy components reenter the rectifying tower for reprocessing, the possibility that the heavy components are carried out in the distillation process is reduced, and the separation precision is improved.

Next, by adjusting the first temperature adjusting assembly 400, the temperature of the liquid in the extractor 310 is increased to T3, where T3 is Tb multiplied by the floating coefficient K1. By adjusting the second temperature adjusting 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. T3 and T4 are both between the boiling point Ta of the heavy component A and the boiling point Tb of the light component B, and the first and second temperature regulating components are used for heating the condensate to keep the condensate at a temperature level which is close to or higher than the boiling point of the light component and is smaller than the boiling point of the heavy component, so that the probability that the light component B is condensed in the process of contacting with reflux liquid or flowing through the overflow pipe 330 is reduced, invalid reflux and light component loss are effectively avoided, and the light component removing efficiency is improved.

Finally, by continuing the 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 rectifying tower completes the light component removal process.

In summary, the method has the core technical effects that the high-temperature condensate is utilized to flush steam, heavy components carried in the steam are effectively recovered, and the temperature of the reflux liquid is controlled through the temperature adjusting component so as to avoid the premature condensation of light components, thereby realizing the efficient and accurate separation of the light components and the heavy components, and obviously improving the purity and the process adaptability of the precursor for the semiconductor.

The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.

The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.

Claims (15)

1. Precursor rectifying device for semiconductor, including heat exchange assembly (100), characterized by still including:

The distribution assembly (200), the distribution assembly (200) comprises a distribution pipe body (210), and a connecting hole (220) for conveying steam by the rectifying tower is formed in the bottom of the distribution pipe body (210);

The liquid collecting assembly (300) is arranged between the distribution pipe body (210) and the heat exchange assembly (100), the liquid collecting assembly (300) comprises a collector (310) used for collecting liquid generated by condensation of the heat exchange assembly (100), a base plate (320) is arranged at the bottom of the collector (310), an overflow pipe (330) and a plurality of gas-phase flow pipes (340) are arranged on the base plate (320), the gas-phase flow pipes (340) are communicated with the collector (310) and the distribution pipe body (210), one end of the overflow pipe (330) extends into the collector (310) and forms a liquid collecting space (380) with the side wall surface of the collector (310), one end of the overflow pipe (330) extends into the collector (310) and is provided with an overflow port (331), and the other end extends into the distribution assembly (200) and is located above the connecting hole (220), so that condensate can be in contact with steam from the rectifying tower in the distribution pipe body (210), and heavy component substances in the flushing steam are realized.

2. The precursor rectification apparatus for semiconductor according to claim 1, wherein said overflow pipe (330) is located at a central position of said base plate (320), and a plurality of said gas phase flow tubes (340) are provided around said overflow pipe (330).

3. The precursor rectification apparatus for semiconductor as recited in claim 1, wherein said overflow port (331) is located at a height exceeding said base plate (320) such that liquid in said extractor (310) enters said overflow pipe (330) through said overflow port (331) when a certain amount is accumulated.

4. The precursor rectification apparatus for semiconductor according to claim 1, wherein said overflow pipe (330) is disposed coaxially with said connection hole (220), an inner diameter of said overflow pipe (330) is not smaller than a diameter of said connection hole (220), and a liquid in said overflow pipe (330) flows back into the rectification column through said connection hole (220).

5. The precursor rectification apparatus for semiconductor according to claim 1, wherein a first flange (230) for connecting a rectification column is provided at a bottom of said distribution pipe body (210), and said connection hole (220) is provided on said first flange (230).

6. The precursor rectification apparatus for semiconductor according to claim 1, wherein an air outlet hole (341) is formed at one end of the gas phase flow tube (340) extending into the extractor (310), an air inlet hole (342) is formed at the other end of the gas phase flow tube (340), and the air inlet hole (342) is flush with the bottom surface of the base plate (320).

7. The precursor rectification apparatus for semiconductor as recited in claim 6, wherein a distance from said overflow port (331) to said substrate (320) is smaller than a distance from said gas outlet hole (341) to said substrate (320).

8. The precursor rectification apparatus for semiconductor as recited in claim 1, wherein said base plate (320) is integrally formed with a side wall surface of said extractor (310).

9. The precursor rectification device for semiconductors according to claim 1, wherein a second flange (350) is arranged on an outer side wall surface of the bottom of the liquid collecting assembly (300), the second flange (350) protrudes out of an outer side wall surface of the liquid collecting assembly (300), a third flange (240) is arranged on an outer side wall surface of the top of the distribution assembly (200), the third flange (240) protrudes out of an outer side wall surface of the distribution assembly (200), and the second flange (350) is connected with the third flange (240) in an equal diameter and matched mode so as to connect the liquid collecting assembly (300) with the distribution assembly (200).

10. The precursor rectifying device for a semiconductor according to claim 1, further comprising a first temperature adjusting assembly (400), wherein the first temperature adjusting assembly (400) comprises a heating pipe (410) arranged in a side wall of the extractor (310), the heating pipe (410) is wound around the side wall of the extractor (310), a top of the heating pipe (410) is flush with a top of the overflow pipe (330) and is connected with a heat source device for heating the liquid in the extractor (310), and the first temperature adjusting assembly (400) further comprises a first temperature sensor for collecting a temperature of the liquid in the extractor (310).

11. The precursor rectification apparatus for semiconductor as recited in claim 1, further comprising a second temperature regulating assembly connected to said overflow tube (330) for heating the liquid in said overflow tube (330).

12. The precursor rectification apparatus for semiconductor according to claim 6, wherein said gas outlet hole (341) is provided on a side wall surface of said overflow pipe (330) on a side away from said base plate (320), and a top end surface of said gas phase flow pipe (340) on a side away from said base plate (320) is provided in a closed state.

13. The precursor rectification apparatus for semiconductor according to claim 1, wherein a liquid collecting assembly (300) is provided with a liquid collecting port (360), the liquid collecting port (360) is disposed on a side wall surface of the liquid collector (310) close to the substrate (320), a distance from the liquid collecting port (360) to the substrate (320) is smaller than a distance from the overflow port (331) to the substrate (320), and a concentration sensor (370) is disposed on the liquid collecting port (360).

14. A precursor rectification system for semiconductors, comprising a precursor rectification apparatus for semiconductors according to any one of claims 1 to 13, characterized by further comprising a rectification column connected to the distribution assembly (200).

15. A method for rectifying a precursor for a semiconductor, using the precursor rectification system for a semiconductor according to claim 14, characterized by comprising the steps of:

adjusting the temperature of the rectifying tower to be the evaporation temperature T1, wherein the 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 in the rectifying tower;

Adjusting the heat exchange assembly (100) to a condensation temperature T2, wherein T2 is smaller than Tb, and collecting liquid generated by condensation of the heat exchange assembly (100) until the liquid is collected in the extractor (310) and flows into the overflow pipe (330);

Adjusting the first temperature adjusting component (400) until the liquid temperature in the extractor (310) reaches T3, wherein T3 is the Tb floating coefficient K1;

Adjusting the second temperature adjusting component until the temperature of the liquid in the overflow pipe (330) reaches T4, wherein T4 is the Tb floating coefficient K2;

and (3) continuing to evaporate until the concentration of the light component B in the liquid in the extractor (310) reaches a threshold value, and judging that the liquid precursor in the rectifying tower is light.