An electronic grade polysilicon water quenching, crushing, screening and pickling integrated treatment method and device

Abstract

The present application relates to the technical field of electronic grade polysilicon production, and particularly relates to a water quenching, crushing, screening and pickling integrated processing method and device for electronic grade polysilicon, which comprises the following steps: pretreating polysilicon rods to obtain electronic grade segmental material; conveying the segmental material to a water quenching station, cooling the segmental material by high-purity water after heating, so that internal cracks are generated and internal stress is released; then crushing and screening the segmental material to obtain silicon material with different particle sizes under high-purity water spraying; loading qualified silicon material into a basket and binding the weight and batch information; conveying the silicon material into an acid pickling and drying station through airtight transmission, sequentially completing acid pickling, water washing, drying and cooling to obtain finished silicon material; and then automatically matching the weight, packaging and storing the finished silicon material according to the batch information; through process integration, airtight transmission and automatic control, material exposure and manual intervention are reduced, the pollution risk is reduced, and the product cleanliness and quality consistency are improved.

Description

Technical Field

[0001] This invention relates to the field of electronic-grade polysilicon production technology, and in particular to an integrated treatment method and apparatus for water quenching, crushing, screening, and acid washing of electronic-grade polysilicon. Background Technology

[0002] Electronic-grade polysilicon is a fundamental material in the semiconductor industry. Its purity directly affects the performance and yield of products such as chips and discrete devices. In order to meet the stringent requirements of impurity content for nanoscale processes, electronic-grade polysilicon must avoid any form of metal contamination, particle introduction, and environmental cross-contamination during the production process. Therefore, the cleanliness and automation level of post-processing steps such as crushing, screening, pickling, and drying are required to be extremely high.

[0003] Currently, the conventional processing flow for electronic-grade polysilicon is as follows: the silicon rods obtained from reduction are crushed using a mechanical crusher, then screened and boxed, then transferred to a cleaning machine for acid washing and drying, and finally manually bagged and packaged. The above processes are scattered in different equipment, relying on a large amount of manual handling and operation. As a result, the silicon material is very easy to be contaminated with metal impurities, dust and organic matter during multiple transfers and exposures. At the same time, manual operation is inefficient and batch traceability is difficult, making it difficult to meet the semiconductor industry's demand for large-size, high-purity, traceable polysilicon products for large-scale production.

[0004] The information disclosed in this background section is intended only to enhance the understanding of the general background of the invention and should not be construed as an admission or in any way implying that the information constitutes prior art known to those skilled in the art. Summary of the Invention

[0005] This invention provides an integrated treatment method and apparatus for water quenching, crushing, screening, and pickling of electronic-grade polycrystalline silicon, thereby effectively solving the problems in the background art.

[0006] To achieve the above objectives, the technical solution adopted by this invention is: an integrated treatment method for water quenching, crushing, screening, and pickling of electronic-grade polycrystalline silicon, comprising the following steps: Pre-treatment of polycrystalline silicon rods removes carbon heads and poorly shaped parts to obtain electronic-grade segmented material; The electronic-grade segmented material is transported to the water quenching station, heated, and then cooled with high-purity water, causing internal cracks to form inside the silicon rod and releasing internal stress. The water-quenched silicon rod is conveyed to the crushing station and crushed to obtain polycrystalline silicon blocks within a set particle size range; The polycrystalline silicon blocks are conveyed to the screening station and classified and screened under high-purity water spray to obtain multiple sets of qualified silicon materials with set particle sizes. The qualified silicon material is loaded into the material basket according to the specifications. After weighing and binding the batch information, the material basket with the bound batch information is obtained. The material basket is directly transported to the pickling and drying station via a closed conveyor line, and pickling, water washing, drying and cooling are completed in sequence to obtain finished silicon material that meets the requirements of electronic grade purity. Based on the batch and specification information of the material basket, the finished silicon material is automatically weighed and packaged, and then stored in the warehouse after generating a full life cycle traceability label.

[0007] Furthermore, the defective parts of the silicon rod are identified by a visual recognition module or a spectral recognition module, and the defective parts are precisely removed by a laser cutting mechanism or a mechanical cutting mechanism. The waste material after removal is discharged through a dedicated sealed channel.

[0008] Furthermore, in the water quenching station, the heating temperature is 300℃-900℃, the holding time is 10min-90min, the cooling medium is high-purity water, the cooling rate is ≥20-80℃ / s, and the internal cracks generated inside the silicon rod after cooling are microcracks distributed along the grain boundaries, so the silicon rod as a whole remains intact.

[0009] Furthermore, in the screening station, a screening machine with a high-purity polyurethane, PVDF, PTFE or high-purity silica gel plate in contact with the silicon material is used for screening, and the high-purity water or demineralized water used for spraying is carried out synchronously with the screening vibration to remove the micro powder attached to the surface of the silicon material and to use the water film tension to assist in the separation of silicon materials of different particle sizes.

[0010] Furthermore, the screening station adopts a screening machine, which is equipped with at least four discharge ports, corresponding to particle size ranges of 2mm-6mm, 6mm-45mm, 45mm-100mm, and 100mm-150mm respectively.

[0011] Furthermore, the high-purity water or desalinated water used for spraying is used to recover fine silica particles of 0mm-6mm as a byproduct through a collection and filtration system.

[0012] Furthermore, the material basket is equipped with a chip identifier or QR code, and the batch information includes furnace batch number, production time, equipment number, acid batch and packaging bag batch. The material basket is automatically written to and encrypted by a reader / writer.

[0013] Furthermore, the pickling and drying station specifically includes: sequentially performing a first pickling, a second pickling, and a third pickling, followed by at least three stages of water washing, one hot water washing, air-cutting drying, hot air drying, vacuum drying, and cold air cooling; wherein: The first pickling uses a mixed solution of hydrochloric acid, hydrogen peroxide, and high-purity water; Both the second and third acid washes use a mixed solution of hydrofluoric acid and nitric acid; The pickling and drying station is also equipped with an online concentration monitoring instrument and a circulating cooling pipeline. It automatically determines when to replace the acid based on the real-time detected acid concentration or cumulative etching thickness, and replenishes the acid with a new acid through an automatic replenishment system.

[0014] Furthermore, in the first pickling, the mass concentration of hydrochloric acid and hydrogen peroxide is 5%-50%; in the second and third pickling, the mass concentration of hydrofluoric acid is 25%-55%, the mass concentration of nitric acid is 45%-75%, and the volume ratio of hydrofluoric acid to nitric acid is 1:6-1:80.

[0015] This invention also includes an integrated treatment device for water quenching, crushing, screening, and pickling of electronic-grade polycrystalline silicon, the device comprising: The pretreatment unit is used to pretreat polycrystalline silicon rods, remove carbon heads and morphologically defective parts, and obtain electronic-grade segmented materials; The water quenching unit is used to transport the electronic-grade segmented material to the water quenching station, where it is heated and then cooled by high-purity water, causing internal cracks to form inside the silicon rod and releasing internal stress. The crushing unit is used to transport the water-quenched silicon rods to the crushing station and crush them to obtain polycrystalline silicon blocks with a set particle size range. The screening unit is used to transport polycrystalline silicon blocks to the screening station, where they are classified and screened under high-purity water spray conditions to obtain multiple sets of qualified silicon materials with set particle sizes. The basket binding unit is used to load the qualified silicon material into the basket according to the specifications, and after completing the weighing and batch information binding, a material-carrying basket with bound batch information is obtained. A closed conveying unit is used to directly convey the material basket to the pickling and drying station via a closed conveyor line. The pickling and drying unit is used to sequentially complete pickling, water washing, drying and cooling to obtain finished silicon material that meets the requirements of electronic grade purity; The automatic counterweight packaging unit is used to automatically counterweight and package the finished silicon material according to the batch and specification information of the material basket, and then store it in the warehouse after generating a full life cycle traceability label.

[0016] The beneficial effects of this invention are as follows: by organically connecting and integrating post-processing steps such as pretreatment, water quenching, crushing, screening, pickling, drying and packaging, and by achieving continuous processing throughout the entire process through closed transmission, batch information binding and automated control, the exposure, transfer and human contact opportunities of materials during processing can be significantly reduced, the risk of introducing metal impurities, dust and other external pollutants can be reduced, and the cleanliness, purity stability and quality consistency of electronic-grade polycrystalline silicon products can be improved.

[0017] The above description is only an overview of the technical solution of this application. In order to better understand the technical means of this application and to implement it in accordance with the contents of the specification, and to make the above and other objects, features and advantages of this application more obvious and understandable, specific embodiments of this application are given below. Attached Figure Description

[0018] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0019] Figure 1 A flowchart of an integrated water-quenching, crushing, screening, and pickling process for electronic-grade polycrystalline silicon. Figure 2 A flowchart of an integrated water-quenching, crushing, screening, and pickling process for electronic-grade polycrystalline silicon. Figure 3 This is a flowchart of the pickling and drying station. Detailed Implementation

[0020] The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments.

[0021] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. The terminology used in this specification is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and / or" as used herein includes any and all combinations of one or more of the associated listed items.

[0022] Example 1: like Figures 1 to 3 As shown, this application provides an integrated water-quenching, crushing, screening, and pickling treatment method for electronic-grade polycrystalline silicon, the method comprising: S10: Pre-process the polycrystalline silicon rod to remove carbon heads and poorly shaped parts to obtain electronic-grade segmented material; S20: Electronic grade segmented material is transported to the water quenching station, heated and then cooled by high-purity water, causing internal cracks to be generated inside the silicon rod and releasing internal stress; S30: The water-quenched silicon rod is conveyed to the crushing station and crushed to obtain polycrystalline silicon blocks with a set particle size range; S40: The polycrystalline silicon block is conveyed to the screening station and classified and screened under the condition of high-purity water spray to obtain multiple sets of qualified silicon materials with set particle sizes. S50: Load qualified silicon material into the material basket according to specifications, and after completing the weighing and batch information binding, obtain the material basket with the bound batch information; S60: The material basket is directly transported to the pickling and drying station via a closed conveyor line. The entire process is carried out without manual intervention or intermediate offline transfer. Pickling, washing, drying and cooling are completed in sequence to obtain finished silicon material that meets the requirements of electronic grade purity. S70: Based on the batch and specification information of the material basket, automatically weigh and package the finished silicon material, generate a full life cycle traceability label, and then store it in the warehouse.

[0023] Specifically, the polycrystalline silicon rod is first pretreated by removing carbon heads and morphologically defective parts containing bubbles, inclusions, or structural defects using automated cutting equipment, including diamond wire cutting devices or sawing devices. After cutting, electronic-grade segments with dimensions meeting subsequent processing requirements are obtained. The segments are then transported to the water quenching station via a closed conveyor system, which includes a sealed conveying channel and a dustproof sealing structure to prevent external contamination. In the water quenching station, the segments are heated by a heating device to bring their overall temperature to the process control range and maintain temperature uniformity. The heating device includes a resistance furnace or induction heating furnace, and a temperature detection unit is configured to monitor different positions of the silicon rod in real time. After heating, the rod immediately enters the cooling zone for rapid cooling with high-purity water. Cooling is achieved through spraying or immersion, and the cooling rate is controlled by adjusting the water flow rate, spray distribution, and circulation status. This creates a temperature gradient between the surface and interior of the silicon rod, generating thermal stress. This causes cracks to preferentially propagate along grain boundaries, forming microcrack structures, while preventing the formation of through cracks that could lead to overall fragmentation.

[0024] After water quenching, the silicon rods enter the crushing station through a closed conveying system. The crushing station is equipped with a closed crushing chamber and a dust removal structure. The crushing equipment uses a jaw crusher or a roller crusher to crush the silicon rods into polycrystalline silicon blocks within a preset particle size range. The crushed material enters the screening station, where it is graded through a multi-layer screen structure. The screens are made of high-purity polyurethane, PVDF, PTFE, or high-purity silicone. Simultaneously, high-purity water is sprayed during the screening process. The spraying and vibration are linked through a control system to form a continuous water film on the screen surface. The water flow removes the attached micro-powder and changes the particle motion state through the surface tension of the water film, thereby improving the separation effect of particles of different sizes.

[0025] After screening, silicon materials of different particle sizes are loaded into baskets by an automatic basket loading system. The basket loading system includes a weighing unit and a control unit. During the loading process, the weight information is collected in real time, and the particle size information, source batch and process parameters are bound to the basket to form a uniquely identified material basket. Then, the basket is transported to the pickling and drying station by a closed conveying system. The conveying system adopts a closed track or automatic guided vehicle structure to achieve no manual intervention and no intermediate transfer throughout the process.

[0026] In the pickling and drying station, the material basket undergoes pickling, washing, drying and cooling processes in sequence. The pickling process uses a multi-stage pickling structure to remove the surface oxide layer and metal impurities. The washing process uses multi-stage high-purity water to remove residual acid. The drying process uses hot air or vacuum to remove moisture. Finally, the silicon material is cooled to reach a stable state. Finally, according to the batch and specification information bound to the material basket, the finished silicon material is quantitatively packaged by an automatic counterweight system, and a traceability label containing process parameter information is generated before it is stored in the warehouse.

[0027] By organically linking and integrating post-processing steps such as pretreatment, water quenching, crushing, screening, pickling, drying, and packaging, and achieving continuous processing throughout the entire process through closed transmission, batch information binding, and automated control, this technology significantly reduces the exposure, transfer, and human contact opportunities of materials during processing. It also lowers the risk of introducing metal impurities, dust, and other exogenous contaminants, thus improving the cleanliness, purity stability, and quality consistency of electronic-grade polysilicon products. Simultaneously, this technical solution enhances the automation level and production continuity of the post-processing, reduces manual operation intensity and human error, and improves batch management and full-process traceability capabilities. This better meets the semiconductor industry's requirements for high purity, large-scale production, and quality traceability of electronic-grade polysilicon products.

[0028] As a preferred embodiment of the above, in step S10, the defective parts of the silicon rod are identified by a visual recognition module or a spectral recognition module, and the defective parts are precisely removed by a laser cutting mechanism or a mechanical cutting mechanism. The waste material after removal is discharged through a dedicated sealed channel.

[0029] Specifically, the silicon rod is transported to an identification station, where an identification module is installed. This module can be either a visual identification module or a spectral identification module. The visual identification module uses an industrial camera to capture images of the silicon rod surface and combines image processing algorithms to analyze features such as color differences, cracks, bubbles, and structural anomalies to determine the location and extent of defects. The spectral identification module scans the silicon rod surface spectrally and identifies impurity-rich or abnormal areas based on differences in optical response in different regions. The identification results are processed by the control system to generate location information of the defects and transmitted to the cutting mechanism. Subsequently, in the cutting station, the silicon rod is precisely cut according to the location information. The cutting mechanism can be a laser cutting mechanism or a mechanical cutting mechanism. The laser cutting mechanism uses a focused laser beam to perform non-contact cutting of the target area to achieve high precision, while the mechanical cutting machine... The cutting mechanism can employ diamond wire cutting or sawing to achieve stable removal, and the control system can adjust the cutting path based on the identification results to reduce effective silicon material loss while ensuring the removal of defective parts. In another specific implementation, the identification module can use a multi-angle visual acquisition structure to perform surround detection on the silicon rod, or use a combination of visual recognition and spectral recognition to improve identification accuracy. At the same time, the cutting mechanism can also use a combination of laser and mechanical methods to balance accuracy and efficiency. After the cutting is completed, the generated waste is discharged through a dedicated closed channel. Specifically, a closed collection device is set up in the cutting area, and the waste is introduced into the collection unit through a negative pressure conveying or closed transmission structure, thereby avoiding waste leakage and mixing with qualified silicon material. This achieves continuous and closed processing of defective part identification, cutting, and waste discharge, improving the automation level and cleanliness control capabilities of the pre-processing stage.

[0030] In this embodiment, in step S20, in the water quenching station, the heating temperature is 300℃-900℃, the holding time is 10min-90min, the cooling medium is high-purity water, the cooling rate is ≥20-80℃ / s, and the internal cracks generated inside the silicon rod after cooling are microcracks distributed along the grain boundaries, and the silicon rod as a whole remains intact.

[0031] Specifically, the pre-treated segmented silicon rods are transported to a heating device for heating. This device can be a resistance furnace or an induction furnace. A control system regulates the heating temperature and holding time to ensure the silicon rod reaches the set temperature range and achieves internal temperature uniformity. After holding, the silicon rod is rapidly transferred to a cooling zone using high-purity water as the cooling medium. Rapid cooling is achieved through spraying or immersion methods, and the cooling rate is adjusted by regulating the water flow intensity, flow distribution, and circulation to meet set requirements. This creates a temperature gradient between the surface and interior of the silicon rod, generating thermal stress and inducing the formation of microcracks extending along grain boundaries, while preventing through-cracks and keeping the silicon rod macroscopically intact. In another specific embodiment, a temperature monitoring unit can be installed in the heating zone to monitor different locations on the silicon rod. Real-time temperature measurement and feedback adjustment of heating power reduce internal temperature differences. Simultaneously, flow and temperature control devices are installed in the cooling zone to stabilize cooling conditions, thereby improving the consistency of microcrack formation. In another specific embodiment, a staged cooling method can be adopted, i.e., first achieving rapid cooling through high-intensity cooling, and then achieving uniform cooling through gentler cooling, to further control crack morphology. Specifically, spray cooling rapidly cools the surface of the silicon rod while maintaining a relatively high internal temperature, thereby forming stress concentration and generating a microcrack network at grain boundaries. Alternatively, immersion cooling with adjusted water flow can obtain microcrack structures with different distribution characteristics. Through these methods, while maintaining the overall structural integrity of the silicon rod, a microcrack system conducive to subsequent crushing can be constructed inside, thereby reducing crushing energy consumption, improving particle size uniformity, and reducing fine powder generation.

[0032] In step S30, the crushing station uses a jaw crushing process to crush the silicon rod, and the resulting polycrystalline silicon block has a particle size range of 0-150mm.

[0033] As a preferred embodiment of the above, in step S40, a screening machine with a high-purity polyurethane, PVDF, PTFE or high-purity silica gel plate in contact with the silicon material is used for screening in the screening station, and the high-purity water or desalinated water used for spraying is carried out synchronously with the screening vibration, so as to remove the micro powder attached to the surface of the silicon material and use the water film tension to assist in the separation of silicon materials of different particle sizes.

[0034] Specifically, the crushed polycrystalline silicon blocks are conveyed into a screening machine via a closed system. The parts of the screening machine that come into contact with the silicon material are made of high-purity polyurethane, polyvinylidene fluoride (PVDF), polytetrafluoroethylene (PTFE), or high-purity silica gel to avoid metal contamination that may occur with traditional metal parts. The low leaching and corrosion resistance of these materials also meet the cleanliness requirements of electronic-grade polycrystalline silicon. During the screening process, a vibration mechanism drives the screen body to vibrate, causing silicon materials of different sizes to separate on the screen surface and achieve particle size classification. Simultaneously, high-purity water or demineralized water is sprayed during the screening process, and the spraying process is coordinated with the screening vibration process through a control system, forming a uniformly distributed dynamic water film on the screen surface. This water flow washes the silicon surface to remove adhering micro-powder, and utilizes... The surface tension generated by the water film alters the contact state between particles and between particles and the screen surface, causing particles of different sizes to exhibit differentiated motion behaviors under vibration. This assists in achieving more effective particle size separation and reducing fine powder entrainment. In another embodiment, the screening equipment can adopt a multi-layer structure, with each layer of the screen surface using the aforementioned high-purity material, and is combined with a multi-point spray structure to ensure uniform distribution of the water film in each layer. Simultaneously, the vibration parameters and spray state are adjusted through linkage control to adapt to the screening requirements of materials with different particle sizes. In this embodiment, the silicon material rolls on the high-purity polyurethane or PTFE screen surface with vibration, forming a stable water film environment under synchronous spraying. Fine particles are washed away while larger particles are classified, thereby achieving synergistic screening, cleaning, and cleanliness control, improving screening accuracy and material cleanliness.

[0035] In step S40, a screening machine is used at the screening station. The screening machine is equipped with at least four discharge ports, which correspond to particle size ranges of 2mm-6mm, 6mm-45mm, 45mm-100mm, and 100mm-150mm, respectively.

[0036] Specifically, the screening machine is equipped with at least four discharge ports to achieve multi-stage particle size separation of polycrystalline silicon particles. The screening machine employs a multi-layer screen structure, with screen surfaces of different apertures arranged sequentially from top to bottom. The crushed polycrystalline silicon material moves and stratifies along the screen surface under vibration. Silicon materials of different particle size ranges pass through their corresponding screen holes and enter their respective discharge channels, exiting through their corresponding discharge ports. Each discharge port corresponds to silicon materials in different particle size ranges, thus achieving multi-stage grading output within a single device. Each discharge port is connected to the main body of the screening machine through an independent, sealed flow guiding structure, keeping silicon materials of different particle sizes isolated during discharge to prevent mixing. Each port can be connected to a corresponding conveying device or collection container to achieve direct connection with subsequent basket loading or processing steps. The high-purity material sieve surface and synchronous spray structure allow for simultaneous removal of surface micro-powder and cleaning of silicon materials of various particle sizes during the sieving process. In another embodiment, the number of sieve layers and the size of the sieve holes can be adjusted according to actual needs to achieve fine grading of different particle size ranges. Online detection devices can be installed at each discharge port to feed back particle size distribution information to the control system for dynamic optimization of sieving parameters. In this embodiment, after the polycrystalline silicon material enters the sieving machine, it is separated step by step through multiple sieve surfaces. Silicon materials of different particle sizes are output from their respective discharge ports and transported to their respective material baskets or subsequent processing units through independent channels. At the same time, it is linked with the automatic weighing and batch binding system to achieve continuous and automated connection of sieving, diversion and subsequent processing, thereby improving grading accuracy and production efficiency.

[0037] As a preferred embodiment of the above embodiments, the high-purity water or desalinated water used for spraying recovers fine silica particles of 0mm-6mm as a byproduct through a collection and filtration system. Specifically, a closed water collection structure is set below the screening machine to collect the spray water and fine particle mixture generated during the screening process, and transports it to the filtration system through a closed pipeline. The filtration system may include multi-stage filtration units, which use filter media of different filtration precision to classify and retain particles in the mixture, so that the fine silica particles can be effectively separated. The separated fine silica particles are collected after dehydration, while the filtered water is returned to the spraying system for recycling. In another embodiment, the recovery filtration system may adopt a structure combining sedimentation and filtration, that is, firstly, sedimentation... The settling unit causes larger density particles to settle, and the remaining suspended particles are then retained by the filtration unit to improve recovery efficiency. In another embodiment, the filtration system can use a multi-stage filter media combination to adapt to the separation requirements of particles of different sizes. In this embodiment, the water containing fine silica particles generated during the screening process is collected in a closed water collection tank and then enters the filtration system. Fine silica particles are obtained as a byproduct through step-by-step filtration and dehydration, and the treated water is reused in the spraying process, thus forming a closed-loop circulation system. Through the above methods, not only can the effective recovery and resource utilization of fine silica particles be achieved, but also the accumulation of fine particles in the system can be reduced, the stability of the screening process can be maintained, and the cleanliness and economy of the overall process can be improved.

[0038] In this embodiment, in step S50, the material basket is equipped with a chip identifier or QR code. The batch information includes furnace batch number, production time, equipment number, acid batch, and packaging bag batch. The material basket is automatically written to and encrypted by a reader / writer. By setting an information identification unit on the material basket, the batch information of polysilicon throughout the entire process is automatically bound and encrypted. Specifically, an identification carrier is fixedly set on the material basket. The identification carrier can be an embedded chip identifier or an attached QR code. The chip identifier can be a readable and writable electronic unit such as an RFID tag, and the QR code is used to carry the corresponding encoded information. After the basket is loaded, it enters the information writing station. The reader / writer set on the conveying path automatically identifies the identification carrier and writes the batch information into it. The batch information includes key data such as furnace batch number, production time, equipment number, acid batch, and packaging bag batch. This establishes a correspondence between the material basket and the entire process parameters. During the writing process, the control system encrypts the data before storage to improve data security and prevent tampering. In subsequent workstations, the reader continuously reads and verifies the identification information, enabling real-time tracking of the material basket's flow path and processing status. In another embodiment, the identification carrier can use a combination of chip identification and QR codes to balance encrypted storage and rapid identification. Readers can be deployed at multiple key workstations to achieve multi-point information verification and process linkage control. In a specific example, after the material basket is loaded with silicon, it enters the writing area, where the reader automatically encrypts and writes the corresponding batch information into the chip. This information is continuously read and recorded at subsequent processing workstations, forming a complete data chain. Scanning the QR code allows for quick access to basic information for on-site verification. Through this method, automated batch information binding and full-process traceability management are achieved in the polysilicon processing process, effectively avoiding batch confusion, improving data security, and enhancing the automation and management level of the production process.

[0039] As a preferred embodiment of the above embodiment, in step S60, the pickling and drying station specifically includes: sequentially performing a first pickling, a second pickling, and a third pickling, followed by at least three stages of water washing, a single hot water washing, air-cutting drying, hot air drying, vacuum drying, and cold air cooling; wherein: The first pickling uses a mixed solution of hydrochloric acid, hydrogen peroxide, and high-purity water; Both the second and third acid washes use a mixed solution of hydrofluoric acid and nitric acid; The pickling and drying station is also equipped with online concentration monitoring instruments and circulating cooling pipes. It automatically determines when to replace the acid based on the real-time detected acid concentration or cumulative etching thickness, and replenishes the acid with new acid through an automatic replenishment system.

[0040] In a preferred embodiment of the above, the mass concentrations of hydrochloric acid and hydrogen peroxide are both 5%-50% in the first pickling; the mass concentrations of hydrofluoric acid and nitric acid are 25%-55% and 45%-75% in the second and third pickling, respectively, with a volume ratio of hydrofluoric acid to nitric acid of 1:6-1:80. In this embodiment, the concentrations of hydrofluoric acid and nitric acid are 40%wt and 50%wt in the second and third pickling, respectively. Through a continuous combination of multi-stage pickling, multi-stage washing, and multi-stage drying, coupled with online monitoring and automatic liquid replenishment control, the polycrystalline silicon surface... The efficient removal of surface impurities and stable process operation are achieved through the following steps: After the material basket is conveyed into the pickling and drying station via a closed system, it undergoes a first pickling, a second pickling, and a third pickling process sequentially. The first pickling uses a mixed solution of hydrochloric acid, hydrogen peroxide, and high-purity water to remove surface metal ions and organic contaminants. The second and third picklings use a mixed solution of hydrofluoric acid and nitric acid to further etch the silicon surface and remove the oxide layer and deep impurities. Automatic conveying and transition structures connect the different pickling stages to minimize cross-contamination of acid solutions. After pickling, the material basket is then... The silicon material undergoes a multi-stage water washing process to remove residual acid, followed by a hot water wash to enhance the cleaning effect. This is followed by air drying, hot air drying, and vacuum drying, using different drying methods to synergistically remove surface and internal residual moisture. Finally, cold air cooling restores the silicon material to a stable state. Throughout this process, the acid washing and drying station is equipped with online concentration monitoring instruments and circulating cooling pipes to monitor and control the acid concentration and temperature in real time. The acid state is assessed based on the throughput or etching degree, and an automatic replenishment system replenishes or replaces acid when set conditions are met, maintaining the acid within a stable range. In another embodiment, the acid washing process can employ a multi-tank structure to adapt to different cycle times, and the water washing can use a counter-current method to improve water utilization efficiency. Drying stage parameters can be adjusted in conjunction to optimize the effect. In this embodiment, the material basket undergoes three stages of acid washing, multi-stage water washing, and multi-stage drying, with online monitoring and automatic replenishment maintaining process stability throughout the process. This achieves continuous and precise control of the acid washing and drying process, improving the cleanliness, consistency, and production efficiency of the silicon material.

[0041] In step S70, the full lifecycle traceability label contains an encrypted QR code containing the following information: furnace batch number, production time, water quenching parameters, crushing parameters, sieving particle size range, pickling formula batch, drying temperature, packaging bag batch, and quality inspection data. The label information is associated with the batch information of the material basket, supporting reverse traceability from the finished silicon material to the original silicon rod and production process parameters.

[0042] Example 2: This invention also includes an integrated treatment device for water quenching, crushing, screening, and pickling of electronic-grade polycrystalline silicon, the device comprising: The pretreatment unit is used to pretreat polycrystalline silicon rods, remove carbon heads and morphologically defective parts, and obtain electronic-grade segmented materials; The water quenching unit is used to transport electronic-grade segmented materials to the water quenching station. After being heated, the materials are cooled by high-purity water, which causes internal cracks to be generated inside the silicon rod and releases internal stress. The crushing unit is used to transport the water-quenched silicon rods to the crushing station and crush them to obtain polycrystalline silicon blocks with a set particle size range. The screening unit is used to transport polycrystalline silicon blocks to the screening station, where they are classified and screened under high-purity water spray conditions to obtain multiple sets of qualified silicon materials with set particle sizes. The basket binding unit is used to load qualified silicon material into the basket according to specifications. After weighing and binding the batch information, a material-carrying basket with bound batch information is obtained. The closed conveying unit is used to directly transport the material basket to the pickling and drying station via a closed conveyor line, without manual intervention or intermediate offline transfer. The pickling and drying unit is used to sequentially complete pickling, water washing, drying and cooling to obtain finished silicon material that meets the requirements of electronic grade purity; The automatic counterweight packaging unit is used to automatically counterweight and package finished silicon materials according to the batch and specification information of the material basket, and then store them in the warehouse after generating a full life cycle traceability label.

[0043] The adjustment device described above in this invention can effectively realize the integrated treatment method of water quenching, crushing, screening and pickling of electronic-grade polycrystalline silicon. The technical effects it can achieve are as described in the above embodiments, and will not be repeated here.

[0044] Similarly, the above-mentioned optimization schemes for the device can also achieve the optimization effects corresponding to the methods in Embodiment 1, which will not be repeated here.

[0045] Although this application has been described in conjunction with specific features and embodiments, it is obvious that various modifications and combinations can be made thereto without departing from the spirit and scope of this application. Accordingly, this specification and accompanying drawings are merely exemplary illustrations of the application as defined herein, and are to be considered as covering any and all modifications, variations, combinations, or equivalents within the scope of this application. Clearly, those skilled in the art can make various alterations and modifications to this application without departing from its scope. Thus, if such modifications and modifications fall within the scope of this application and its equivalents, this application intends to include such modifications and modifications.

Claims

1. A method for integrated water quenching, crushing, screening, and pickling of electronic-grade polycrystalline silicon, characterized in that, The method includes: Pre-treatment of polycrystalline silicon rods removes carbon heads and poorly shaped parts to obtain electronic-grade segmented material; The electronic-grade segmented material is transported to the water quenching station, heated, and then cooled with high-purity water, causing internal cracks to form inside the silicon rod and releasing internal stress. The water-quenched silicon rod is conveyed to the crushing station and crushed to obtain polycrystalline silicon blocks within a set particle size range; The polycrystalline silicon blocks are conveyed to the screening station and classified and screened under high-purity water spray to obtain multiple sets of qualified silicon materials with set particle sizes. The qualified silicon material is loaded into the material basket according to the specifications. After weighing and binding the batch information, the material basket with the bound batch information is obtained. The material basket is directly transported to the pickling and drying station via a closed conveyor line, and pickling, water washing, drying and cooling are completed in sequence to obtain finished silicon material that meets the requirements of electronic grade purity. Based on the batch and specification information of the material basket, the finished silicon material is automatically weighed and packaged, and then stored in the warehouse after generating a full life cycle traceability label.

2. The integrated water quenching, crushing, screening, and pickling treatment method for electronic-grade polycrystalline silicon according to claim 1, characterized in that, Defective parts of the silicon rod are identified by a visual recognition module or a spectral recognition module, and the defective parts are precisely removed by a laser cutting mechanism or a mechanical cutting mechanism. The waste material after removal is discharged through a dedicated sealed channel.

3. The integrated water quenching, crushing, screening, and pickling treatment method for electronic-grade polycrystalline silicon according to claim 1, characterized in that, In the water quenching station, the heating temperature is 300℃-900℃, the holding time is 10min-90min, the cooling medium is high-purity water, the cooling rate is ≥20-80℃ / s, and the internal cracks generated inside the silicon rod after cooling are microcracks distributed along the grain boundaries, and the silicon rod as a whole remains intact.

4. The integrated water quenching, crushing, screening, and pickling treatment method for electronic-grade polycrystalline silicon according to claim 1, characterized in that, In the screening station, a screening machine with a high-purity polyurethane, PVDF, PTFE or high-purity silica gel plate in contact with the silicon material is used for screening. The high-purity water or demineralized water used for spraying is carried out synchronously with the screening vibration to remove the micro powder attached to the surface of the silicon material and to use the water film tension to assist in the separation of silicon materials of different particle sizes.

5. The integrated water-quenching, crushing, screening, and pickling treatment method for electronic-grade polycrystalline silicon according to claim 4, characterized in that, The screening station uses a screening machine, which has at least four discharge ports, corresponding to particle size ranges of 2mm-6mm, 6mm-45mm, 45mm-100mm, and 100mm-150mm respectively.

6. The integrated water quenching, crushing, screening, and pickling treatment method for electronic-grade polycrystalline silicon according to claim 4, characterized in that, The high-purity water or desalinated water used for spraying is collected and filtered to recover fine silica particles of 0mm-6mm as a byproduct.

7. The integrated water quenching, crushing, screening, and pickling treatment method for electronic-grade polycrystalline silicon according to claim 1, characterized in that, The material basket is equipped with a chip identifier or QR code. The batch information includes furnace batch number, production time, equipment number, acid batch and packaging bag batch. The material basket is automatically written to and encrypted by a reader.

8. The integrated water-quenching, crushing, screening, and pickling treatment method for electronic-grade polycrystalline silicon according to claim 1, characterized in that, The pickling and drying station specifically includes: sequentially performing a first pickling, a second pickling, and a third pickling, followed by at least three stages of water washing, one hot water washing, air-cutting drying, hot air drying, vacuum drying, and cold air cooling; wherein: The first pickling uses a mixed solution of hydrochloric acid, hydrogen peroxide, and high-purity water; Both the second and third acid washes use a mixed solution of hydrofluoric acid and nitric acid; The pickling and drying station is also equipped with an online concentration monitoring instrument and a circulating cooling pipeline. It automatically determines when to replace the acid based on the real-time detected acid concentration or cumulative etching thickness, and replenishes the acid with a new acid through an automatic replenishment system.

9. The integrated water quenching, crushing, screening, and pickling treatment method for electronic-grade polycrystalline silicon according to claim 8, characterized in that, In the first pickling process, the mass concentrations of hydrochloric acid and hydrogen peroxide are both 5%-50%; in the second and third pickling processes, the mass concentrations of hydrofluoric acid and nitric acid are 25%-55% and 45%-75%, respectively, and the volume ratio of hydrofluoric acid to nitric acid is 1:6-1:

80.

10. An integrated treatment device for water quenching, crushing, screening, and pickling of electronic-grade polycrystalline silicon, characterized in that, The device includes: The pretreatment unit is used to pretreat polycrystalline silicon rods, remove carbon heads and morphologically defective parts, and obtain electronic-grade segmented materials; The water quenching unit is used to transport the electronic-grade segmented material to the water quenching station, where it is heated and then cooled by high-purity water, causing internal cracks to form inside the silicon rod and releasing internal stress. The crushing unit is used to transport the water-quenched silicon rods to the crushing station and crush them to obtain polycrystalline silicon blocks with a set particle size range. The screening unit is used to transport polycrystalline silicon blocks to the screening station, where they are classified and screened under high-purity water spray conditions to obtain multiple sets of qualified silicon materials with set particle sizes. The basket binding unit is used to load the qualified silicon material into the basket according to the specifications, and after completing the weighing and batch information binding, a material-carrying basket with bound batch information is obtained. A closed conveying unit is used to directly convey the material basket to the pickling and drying station via a closed conveyor line. The pickling and drying unit is used to sequentially complete pickling, water washing, drying and cooling to obtain finished silicon material that meets the requirements of electronic grade purity; The automatic counterweight packaging unit is used to automatically counterweight and package the finished silicon material according to the batch and specification information of the material basket, and then store it in the warehouse after generating a full life cycle traceability label.

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