A glove box multi-temperature zone RTP sublimation purification integrated system

Abstract

This invention provides an integrated multi-zone RTP sublimation purification system for a glove box, comprising a glove box chamber and a vacuum unit, and a multi-zone RTP sublimation reactor. The multi-zone RTP sublimation reactor is sealed to the glove box chamber via a transition transfer component. The vacuum unit is connected to the multi-zone RTP sublimation reactor via pipelines and is used to evacuate the multi-zone RTP sublimation reactor. The multi-zone RTP sublimation reactor includes a furnace body and a reaction tube, as well as multiple sets of independently arranged rapid heat treatment heating modules arranged along the axial direction of the reaction tube. Through the multi-zone RTP sublimation reactor, which is sealed to the glove box chamber and equipped with a dedicated vacuum unit for independent evacuation, the entire process of oxygen-free and sealed material transfer can be achieved using the glove box, isolating external air from interfering with the sublimation reaction. Furthermore, the multiple independently arranged rapid heat treatment heating modules are arranged along the axial direction of the reaction tube, allowing for individual control of the heating conditions of corresponding sections of the reaction tube.

Description

Technical Field

[0001] This invention relates to the field of chemical equipment technology, specifically to an integrated multi-temperature zone RTP sublimation purification system for a glove box. Background Technology

[0002] Currently, Mo-based solid precursors, represented by molybdenum dioxide (MoO2Cl2) (including but not limited to MoO2Cl2, MoCl5, etc.), are all fine inorganic chemical raw materials and optoelectronic functional precursor materials that are easily hydrolyzed and oxidized. Upon contact with air, they readily react with water vapor and oxygen, causing material deterioration and a decrease in purity. Therefore, their sublimation purification process must be completed in an anhydrous, oxygen-free, high-vacuum, sealed environment. Meanwhile, RTP refers to Rapid Thermal Processing. Rapid thermal processing heating modules use infrared lamp arrays or laser heating sources, capable of raising the corresponding section of the reaction tube to the target temperature within seconds to tens of seconds, achieving rapid heating and cooling.

[0003] Currently, traditional equipment arranges the glove box, vacuum sublimation furnace, and vacuum unit separately. Material transfer requires multiple openings and transfers, and air repeatedly enters the working chamber, making it impossible to guarantee a completely oxygen-free environment. At the same time, ordinary tubular sublimation furnaces use an integral heating structure, with a uniform temperature throughout the furnace body, making it impossible to achieve zoned gradient temperature control, which is difficult to meet the process requirements of segmented sublimation and graded purification of Mo-type solid precursors. Meanwhile, the use of a single transfer channel for materials of various specifications easily leads to cross-contamination and atmospheric disturbance. Furthermore, the accompanying gas purification devices are mostly based on a shutdown-and-regenerate mode, which cannot meet the demands of continuous, large-scale production. Existing split-type equipment suffers from cumbersome processes, low integration, poor temperature control accuracy, and weak continuous operation capability, severely restricting the purification efficiency and finished product quality of such sensitive precursor materials. Summary of the Invention

[0004] The present invention aims to solve the problems mentioned in the background art by providing an integrated multi-temperature zone RTP sublimation purification system for glove boxes.

[0005] The specific technical solution is as follows: An integrated multi-zone RTP sublimation purification system for a glove box includes a glove box chamber and a vacuum unit, and further includes a multi-zone RTP sublimation reactor. The multi-zone RTP sublimation reactor is sealed to the glove box chamber via a transition transfer component. The vacuum unit is connected to the multi-zone RTP sublimation reactor via a pipeline for evacuating the reactor. The multi-zone RTP sublimation reactor includes a furnace body and a reaction tube, as well as multiple sets of independently arranged rapid heat treatment heating modules arranged along the axial direction of the reaction tube. Each set of rapid heat treatment heating modules is fixedly connected to the top of the furnace body, and each rapid heat treatment heating module can independently control and heat the corresponding section of the reaction tube.

[0006] As a preferred embodiment of the present invention, the glove box is provided with a graded independent vacuum material transfer device inside. The graded independent vacuum material transfer device is used to classify and isolate the transfer of materials, avoid the intrusion of outside air into the glove box by materials of different specifications sharing the same channel, stabilize the inert atmosphere inside the glove box, and reduce the purification load of the box. A purification circulation device is provided on one side of the external side of the glove box for alternating purification and regeneration, and continuously adsorbing water vapor, oxygen and organic impurities inside the box.

[0007] As a preferred embodiment of the present invention, the rapid heat treatment heating module includes an infrared lamp array or a laser heating source.

[0008] As a preferred embodiment of the present invention, a forced cooling cooling fan is provided on the surface of the furnace body and between two adjacent sets of rapid heat treatment heating modules, and an observation window is provided on the surface of the furnace body and on one side of the cooling fan.

[0009] As a preferred embodiment of the present invention, the glove box is provided with two sets of interconnected operating chambers on one side, and the bottom of the operating chamber is provided with multiple sets of rollers for supporting materials. The surface of the glove box is provided with a glove operating opening at the position of each set of operating chambers.

[0010] As a preferred embodiment of the present invention, the graded independent vacuum material transfer component includes a feeding buffer chamber, a small part rapid transfer chamber, and a large part conveying transfer chamber, which are disposed inside the other side of the glove box and are divided into non-interfering feeding buffer chamber, small part rapid transfer chamber, and large part conveying transfer chamber. The feeding buffer chamber has an automatic lifting feeding component built in, and the large part conveying transfer chamber has a material conveying support component built in. The feeding buffer chamber, the small part rapid transfer chamber, and the large part conveying transfer chamber are each independently equipped with a vacuum pumping component, an inert gas replenishment component, and a sealed opening and closing door.

[0011] As a preferred embodiment of the present invention, the purification circulation component includes a fan barrel disposed outside the glove box, the fan barrel having multiple sets of purification columns disposed inside, and the fan barrel being connected to the interior of the glove box through a connecting pipe.

[0012] As a preferred embodiment of the present invention, the transition transfer component includes a connecting flange disposed on one side of the glove box, the other end of the connecting flange being connected to the furnace body, and a high-temperature resistant vacuum sealing ring being embedded inside the connecting flange to achieve seamless vacuum sealing connection between the glove box and the furnace body. The connecting flange is internally integrated with a high-vacuum slide gate valve or gate valve for closing after the material transfer is completed, so that the reaction tube and the glove box are gas-tightly isolated.

[0013] As a preferred embodiment of the present invention, the reaction tube is made of high-purity quartz material, and the inner wall of the reaction tube is sprayed with a high-temperature resistant and anti-adhesion coating. The furnace body is enclosed to form a sealed heat-insulating cavity, and the inner wall of the heat-insulating cavity is lined with nano heat-insulating cotton to isolate the heat from each group of rapid heat treatment heating modules and ensure the temperature control accuracy of a single tube section.

[0014] As a preferred embodiment of the present invention, it also includes a controller and an indicator light electrically connected to the signal output terminal of the controller. The controller is electrically connected to the vacuum unit, multiple sets of rapid heat treatment heating modules, graded independent vacuum material transfer components, purification circulation components, and cooling fans. The controller has built-in independent temperature control module, vacuum pressure acquisition module, and timing linkage control module, which are used to uniformly regulate the vacuum degree of the device, the zone heating temperature, the material transfer sequence, and the start and stop of the chamber purification, so as to realize the fully automated linkage operation of the entire process of oxygen-free vacuum transfer of materials, zoned gradient heating and sublimation, and device atmosphere purification.

[0015] The present invention has the following beneficial effects: 1. This invention utilizes a multi-temperature zone RTP sublimation reaction component, which is sealed and connected to the glove box chamber and independently vacuumed by a dedicated vacuum unit. This allows for fully oxygen-free, sealed material transfer within the glove box, isolating external air from interfering with the sublimation reaction. Furthermore, multiple independently arranged rapid heat treatment heating modules are positioned along the axial direction of the reaction tube, allowing for individual control of the heating conditions of corresponding tube sections. This enables independent temperature control of the tubular cavity, adapting to the differentiated, segmented sublimation processing requirements of materials. The entire device integrates sealed material transfer, vacuum environment construction, and zoned heat treatment sublimation functions. The processes are tightly connected, and the integrated structure is compatible with the entire oxygen-free vacuum sublimation process, resulting in high equipment integration and strong operational continuity.

[0016] 2. This invention enables the classified and isolated transfer of materials through a graded independent vacuum material transfer component, avoiding the problems of air backflow and cabin atmosphere pollution caused by sharing transfer channels for materials of different specifications. It can maintain the stability of the inert atmosphere inside the glove box for a long time, reduce the frequency of gas purification in the cabin, reduce the maintenance load of the box purification, and is equipped with a purification circulation component to realize the alternating purification and regeneration operation of the purification structure, continuously removing water vapor, oxygen and organic impurities in the cabin without stopping the machine to carry out purification consumable regeneration operation, ensuring that the glove box can operate continuously for a long time in a closed manner, and is suitable for large-scale continuous material processing conditions.

[0017] 3. This invention splits materials into three independent transfer chambers, enabling specialized transfer of materials according to size and specifications. The transfer operations do not interfere with or affect each other. Each transfer chamber is independently equipped with vacuum, gas replenishment, and sealing opening and closing structures. The opening and closing of a single chamber only replaces the gas inside itself and does not disturb the inert vacuum environment of the main cavity of the glove box. In addition, it is equipped with dedicated feeding and support components, which are suitable for the closed transfer operations of conventional materials, small materials, and large materials respectively. The material transfer adaptability is wider, and the transfer sealing and safety are higher, preventing air from entering and contaminating the materials from the transfer source. Attached Figure Description

[0018] Figure 1 This is a schematic diagram of the furnace body in the integrated glove box multi-temperature zone RTP sublimation purification system provided in an embodiment of the present invention; Figure 2 This is a front view structural diagram of the glove box compartment in the integrated glove box multi-temperature zone RTP sublimation purification system provided in an embodiment of the present invention; Figure 3 This is a partial top view of the glove box compartment in the integrated multi-temperature zone RTP sublimation purification system provided in this embodiment of the invention.

[0019] In the attached image: 100. Furnace body; 101. Reaction tube; 103. Indicator light; 104. Controller; 105. Observation window; 106. Cooling fan; 200. Glove box body; 201. Connecting flange; 202. Glove operating port; 203. Operating chamber; 204. Roller; 205. Large item conveying and transfer chamber; 206. Small item rapid transfer chamber; 207. Feeding buffer chamber; 208. Automatic lifting and feeding assembly; 300, fan casing; 302, connecting pipe. Detailed Implementation

[0020] The technical solution of the present invention will be further described below with reference to the accompanying drawings and specific embodiments.

[0021] The accompanying drawings are for illustrative purposes only and are schematic diagrams, not actual images. They should not be construed as limiting the scope of this application. To better illustrate the embodiments of the present invention, some parts in the drawings may be omitted, enlarged, or reduced, and do not represent the actual dimensions of the product. It is understandable to those skilled in the art that some well-known structures and their descriptions may be omitted in the drawings.

[0022] In the accompanying drawings of the embodiments of the present invention, the same or similar reference numerals correspond to the same or similar components. In the description of the present invention, it should be understood that if terms such as "upper," "lower," "left," "right," "inner," and "outer" indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, they are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, the terms used to describe positional relationships in the drawings are only for illustrative purposes and should not be construed as limiting the present application. For those skilled in the art, the specific meaning of the above terms can be understood according to the specific circumstances.

[0023] In the description of this invention, unless otherwise explicitly specified and limited, the term "connection" or similar designation indicating a connection between components should be interpreted broadly. For example, it can refer to a fixed connection, a detachable connection, or an integral part; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium; it can refer to the internal communication between two components or the interaction between two components. Those skilled in the art can understand the specific meaning of the above terms in this invention based on the specific circumstances.

[0024] Please see Figures 1-3This embodiment provides an integrated multi-temperature zone RTP sublimation purification system for a glove box, including a glove box chamber 200 and a vacuum unit, and a multi-temperature zone RTP sublimation reactor. The multi-temperature zone RTP sublimation reactor is sealed to the glove box chamber 200 via a transition transfer component. The vacuum unit is connected to the multi-temperature zone RTP sublimation reactor via a pipeline for evacuating the reactor. The multi-temperature zone RTP sublimation reactor includes a furnace body 100 and a reaction tube 101, as well as multiple sets of independently arranged rapid heat treatment heating modules arranged axially along the reaction tube 101. Each rapid heat treatment heating module is fixedly connected to the top of the furnace body 100, and each rapid heat treatment heating module can independently control and heat the reaction tube 101. The corresponding pipe section 01 is heated through a multi-temperature zone RTP sublimation reaction component, which is sealed and connected to the glove box chamber 200 and equipped with a dedicated vacuum unit for independent vacuuming. The glove box enables fully oxygen-free and sealed material transfer, isolating external air from interfering with the sublimation reaction. Furthermore, multiple independently arranged rapid heat treatment heating modules are arranged along the axial direction of the reaction tube 101, which can individually control the heating conditions of the corresponding pipe section of the reaction tube 101, achieving independent temperature control of the tubular cavity. This can adapt to the needs of differentiated segmented sublimation processing of materials. The overall device integrates sealed material transfer, vacuum environment construction, and zoned heat treatment sublimation functions. The process is closely connected, and the integrated structure is suitable for the entire oxygen-free vacuum sublimation process. The equipment has a high degree of integration and strong operational continuity.

[0025] The vacuum unit is connected to the exhaust port at the end of the reaction tube 101 of the multi-temperature zone RTP sublimation reaction unit through a high-vacuum bellows and KF flange assembly. A vacuum gauge, bypass valve and vent valve are connected in series on the pipeline to evacuate the inside of the reaction tube 101, measure the vacuum degree and release pressure and backfill with inert gas.

[0026] The glove box 200 is equipped with a graded independent vacuum material transfer unit inside. This unit is used to classify and isolate materials during transfer, preventing outside air from entering the glove box 200 due to different materials sharing the same transfer channel. This stabilizes the inert atmosphere inside the glove box 200 and reduces the purification load on the box. A purification circulation unit is located on one side of the external glove box 200 for alternating purification and regeneration, continuously adsorbing water vapor, oxygen, and organic impurities within the box. The graded independent vacuum material transfer unit allows for the classified and isolated transfer of materials, avoiding air backflow and atmosphere contamination caused by different materials sharing the same transfer channel. This effectively maintains the stability of the inert atmosphere inside the glove box 200, reduces the frequency of gas purification, lowers the purification maintenance load, and enables alternating purification and regeneration operations. The purification circulation unit allows for continuous removal of water vapor, oxygen, and organic impurities without requiring downtime for purification consumable regeneration, ensuring the glove box can operate continuously and in a sealed environment for extended periods, making it suitable for large-scale continuous material processing.

[0027] The rapid heat treatment heating module includes an infrared lamp array or a laser heating source. By selecting an infrared lamp array or a laser heating source as the heat source for the rapid heat treatment heating module, both types of heat sources have a fast heating response speed and high heat radiation concentration, which can quickly complete the heating operation of a local section of the reaction tube 101 with lower heating energy consumption. At the same time, the heat source has high temperature control sensitivity, which is suitable for short-time rapid heat treatment processes. It can accurately match the processing requirements of instantaneous heating and constant temperature sublimation of materials, and is suitable for the sublimation processing of materials with various physical properties.

[0028] The furnace body 100 is equipped with a forced cooling fan 106 on its surface and between two adjacent rapid heat treatment heating modules. An observation window 105 is also provided on the surface of the furnace body 100 and on one side of the cooling fan 106. By arranging the cooling fan 106 between adjacent heating modules, forced cooling can be applied to the connecting area of ​​the furnace body 100, eliminating the problem of residual heat accumulation in adjacent heating areas, assisting in optimizing the temperature control stability of a single tube section, and preventing residual heat from affecting the accuracy of zoned heating. At the same time, the observation window 105 allows direct visual observation of the sublimation form and reaction progress of the material inside the reaction tube 101. The internal working conditions can be monitored without disassembling the furnace body 100, making it convenient for staff to judge the reaction status in real time and reducing the difficulty of equipment inspection and working condition verification.

[0029] The glove box 200 has two interconnected operating chambers 203 on one side. The bottom of each operating chamber 203 has multiple rollers 204 for supporting materials. Each operating chamber 203 has a glove operating port 202 on its surface. The two interconnected operating chambers 203 combine work zoning with chamber connectivity, which can divert manual operation workload and adapt to multi-person collaborative operation. At the same time, the rollers 204 at the bottom of the operating chamber 203 can flexibly support and push materials, reducing friction during manual material handling and lowering the probability of material collision damage. The dedicated glove operating port 202 on the outside allows for manual assistance in fully enclosed conditions. The entire process of material handling, equipment alignment, and chamber maintenance will not disrupt the inert and sealed environment inside the chamber, balancing operational convenience and atmospheric stability.

[0030] The graded independent vacuum material transfer unit includes a feeding buffer chamber 207, a small-item rapid transfer chamber 206, and a large-item conveying transfer chamber 205, located inside the other side of the glove box 200 and divided into three independent feeding buffer chambers: a feeding buffer chamber 207, a small-item rapid transfer chamber 206, and a large-item conveying transfer chamber 205. The feeding buffer chamber 207 has a built-in automatic lifting and feeding assembly 208, and the large-item conveying transfer chamber 205 has a built-in material conveying and supporting assembly. The feeding buffer chamber 207, the small-item rapid transfer chamber 206, and the large-item conveying transfer chamber 205 are each independently equipped with a vacuum extraction assembly, an inert gas replenishment assembly, and a sealed opening and closing door. The system is divided into three independent transfer compartments, enabling materials to be transferred according to their size and specifications without interference or impact on each other. Each transfer compartment is independently equipped with vacuum, gas replenishment, and sealing opening and closing structures. The opening and closing of a single compartment only replaces the gas inside itself and does not disturb the inert vacuum environment of the main cavity of the glove box. It is also equipped with dedicated feeding and support components, which are suitable for the closed transfer of conventional materials, small materials, and large materials respectively. The material transfer adaptability is wider, and the transfer sealing and safety are higher, preventing air contaminants from entering the materials at the source of transfer.

[0031] The purification circulation component includes a fan barrel 300 located outside the glove box 200. Multiple purification columns are installed inside the fan barrel 300. The fan barrel 300 is connected to the inside of the glove box 200 via a connecting pipe 302. By relying on the multiple purification columns mounted on the fan barrel 300, airflow circulation achieves the cyclic adsorption of impurities within the chamber, resulting in uniform purification coverage and balanced removal of water vapor, oxygen, and organic impurities. Furthermore, the fan barrel 300 is directly connected to the inside of the glove box via the connecting pipe 302, simplifying the pipe connection and ensuring smooth airflow circulation. It can achieve full-area airflow circulation purification using fan power, featuring a compact structure that can be installed and adapted without additional modifications to the box, making it suitable for upgrading existing glove box atmospheres.

[0032] The purification column is filled with a composite bed of 3A molecular sieve and palladium catalyst, which is used to alternately adsorb water vapor, oxygen and organic impurities, and can be regenerated online.

[0033] The transition transfer component includes a connecting flange 201 located on one side of the glove box 200. The other end of the connecting flange 201 is connected to the furnace body 100. A high-temperature resistant vacuum sealing ring is embedded inside the connecting flange 201, enabling seamless vacuum sealing between the glove box 200 and the furnace body 100. The glove box and furnace body 100 are standardizedly connected by relying on the connecting flange 201, which is convenient to disassemble and assemble, has strong connection stability, and the high-temperature resistant vacuum sealing ring embedded inside can seal the flange connection gap, taking into account both high temperature resistance and vacuum sealing performance. It can resist the high temperature conducted by heating operations, avoid the aging and failure of the sealing components, and completely prevent outside air from entering the cavity from the connection gap, ensuring the vacuum tightness of the entire process of material transfer and sublimation, and improving the service life of the entire device.

[0034] The connecting flange 201 also integrates a high-vacuum gate valve or gate valve, which is used to close after the material transfer is completed, so that the reaction tube 101 is airtightly isolated from the glove box 200, thereby allowing the vacuum unit to independently evacuate the reaction tube 101 without affecting the inert atmosphere in the glove box.

[0035] The reaction tube 101 is made of high-purity quartz material. The inner wall of the reaction tube 101 is coated with a high-temperature resistant and anti-adhesion coating. The furnace body 100 forms a sealed heat-insulating cavity, and the inner wall of the heat-insulating cavity is lined with nano-insulation cotton to prevent heat from flowing between the various rapid heat treatment heating modules, ensuring the temperature control accuracy of each tube section. The high-purity quartz material reaction tube 101 has good vacuum resistance and stable chemical properties, and will not react chemically with the materials during the sublimation process, ensuring the purity of the finished product. At the same time, the high-temperature resistant and anti-adhesion coating on the inner wall can prevent the sublimated materials from sticking to the tube wall at high temperatures, simplifying the tube wall cleaning and equipment maintenance procedures. The nano-insulation cotton inside the furnace body 100 can isolate heat conduction between sections, prevent heat from flowing between adjacent heating sections, ensure independent temperature control of each tube section without interference from the surrounding temperature, and improve the accuracy of zoned temperature control.

[0036] Among them, the high-temperature resistant and anti-adhesion coating is preferably a boron nitride suspension high-temperature resistant coating.

[0037] The system also includes a controller 104 and indicator lights 103 electrically connected to the signal output of the controller 104. The controller 104 is electrically connected to the vacuum unit, multiple rapid heat treatment heating modules, graded independent vacuum material transfer components, purification circulation components, and cooling fan 106. The controller 104 has a built-in independent temperature control module, vacuum pressure acquisition module, and timing linkage control module, which are used to uniformly regulate the vacuum degree of the device, the zone heating temperature, the material transfer sequence, and the start and stop of the chamber purification. This enables fully automated linkage operation of the entire process of oxygen-free vacuum transfer of materials, zoned gradient heating and sublimation, and device atmosphere purification. By autonomously matching the operating parameters of the entire process of material transfer, vacuum pumping, zoned heating, heat dissipation control, and atmosphere purification, the system achieves sequential linkage and coordination of each process without the need for manual step-by-step control and intervention. It completes the automated operation of oxygen-free transfer, zoned sublimation, and atmosphere purification in a closed loop, reducing the probability of human error. In addition, the indicator lights 103 provide visual feedback on the operating status of the equipment. When the equipment is abnormal, it can promptly prompt the operation and maintenance personnel to handle it, reducing the risk of operational failure and improving the overall safety and efficiency of the device.

[0038] It is worth noting that the controller 104 of this invention incorporates a multi-temperature zone RTP sublimation comprehensive efficiency control model, and its control equation is as follows: ; The definitions of each key factor are as follows: (1) Sublimation driving factors: ; When the ambient pressure is higher than or equal to the saturated vapor pressure, the contribution of this temperature range is forced to zero to avoid negative contributions interfering with the overall efficiency.

[0039] (2) Synergistic heat-promoting factor of heating-heat preservation: This application abandons the limitation of traditional methods that only consider the heating rate, and introduces the effective heat accumulation equivalent. The transient effect of rapid heating and the sustained effect of constant temperature preservation are unified and quantified into a thermal driving force: ; Among them, effective heat accumulation equivalent Defined as: ; : Characterizes the total temperature rise during the heating phase (unit: K); : Characterizes the isothermal holding time of the material at the target temperature in this temperature range (unit: s); : Equivalent temperature rise conversion coefficient for heat preservation time (unit: K / s), determined by the sublimation activation energy and diffusion characteristics of the material.

[0040] This definition ensures that when the material enters the isothermal stage... At that time, long-term heat preservation can still pass The continuous accumulation of thermal driving force makes It gradually approaches 1, truly reflecting the physical essence of isothermal sublimation.

[0041] (3) Temperature gradient coupling correction factor: ; in, Gradient-driven sensitivity coefficient ( ), Thermal stress penalty coefficient ( When the temperature difference is moderate, the driving force of the molecule increases; when the temperature difference is too large, the quadratic term in the denominator increases rapidly. Attenuation precisely matches the physical constraints that cause thermal stress damage due to excessive temperature difference.

[0042] (4) Boundary conditions: For the final temperature zone Because there is no subsequent temperature range, it is defined as .

[0043] Example application scenarios: The reaction tube consists of four temperature zones: preheating, sublimation, cooling, and collection. The material is high-purity quartz, and the thermal stress penalty coefficient is [not specified]. .

[0044] Given conditions: Environmental pressure ; Saturated vapor pressure in each temperature zone: , , , ; Kinetic coefficients: , , , ; Thermal insulation equivalent coefficient: , , , ; Material weights: .

[0045] Calculation process: Temperature Zone 1 (Preheating Section): ; ; ; ; Contribution Item 1 = .

[0046] Temperature Zone 2 (Sublimation Section): ; ; ; ; Contribution Item 2 = .

[0047] Temperature Zone 3 (Cooling Section): ; ; ; ; Contribution item 3 = .

[0048] Temperature Zone 4 (Collection Section, Final Section): ; ; ; ; (Boundary conditions); Contribution 4 = .

[0049] Overall efficiency: (i.e., 2.455%).

[0050] Technical effects: All index items middle, and The product of is strictly dimensionless, satisfying the basic legality of physical equations.

[0051] By introducing and This completely overcomes the shortcomings of traditional models that rely solely on heating rate for evaluation accuracy; during optimization, it can reasonably allocate heating power and holding time, significantly improving the efficiency evaluation accuracy of the long-term isothermal sublimation stage.

[0052] As the temperature difference changes non-monotonically (increasing first and then decreasing), the controller will automatically avoid excessively large temperature gradients when optimizing the heating gradient. The interval achieves a dynamic optimal balance between directional migration and equipment safety.

[0053] Clearly define the final paragraph This makes the equation applicable to any temperature range. All of them possess mathematical closure and support modular expansion such as multi-segment collection segments.

[0054] The controller is modified When optimizing the objective function, it will not be affected by Instantaneous fluctuations produce negative efficiency ( (Clamping), and will not cause equipment damage due to blindly pursuing excessively large temperature differences ( (Punishment), and will not misjudge the process endpoint due to neglecting the heat preservation time, so that the automated linkage operation is highly close to the real physical and chemical process window.

[0055] Working principle and process: Step 1: Parameter Initialization and Calibration: Operators retrieve pre-calibrated data , , (in and (Determined by a combined isothermal weight loss and heating weight loss experiment), record the target temperature and heating time for each temperature zone. Insulation time Material weights System parameters can be saved with a single click.

[0056] Step Two: Real-time Data Acquisition During operation: The vacuum pressure acquisition module measures pressure in real time. Independent temperature control modules monitor the actual temperature of each temperature zone and calculate the real-time heating rate. Cumulative temperature rise Duration of heat preservation and adjacent temperature difference .

[0057] Step 3: Real-time calculation of efficiency correction: The controller 104 substitutes the collected data into the correction equation and outputs the result in real time. Indicator light 103 according to Deviation from the preset safety threshold is visualized using three colors (green / yellow / red) to intuitively reflect the effectiveness of the current process.

[0058] Step 4: Safety Constraint Closed-Loop Optimization: Sequential linkage constraint module to maximize The goal, but also limited by The penalty clause in the calculation. When the temperature difference between adjacent elements exceeds the material's tolerance threshold (e.g., the maximum allowable temperature difference for a quartz tube is 250K), even if the heating power is increased, On the contrary, because The power decreases due to attenuation. Therefore, the controller automatically adjusts the power of each heating module and controls the start and stop of the cooling fan 106 to bring the system to its optimal state. The range ensures both the directional migration rate and automatically avoids stress risks. Simultaneously, the controller optimizes... , and The ratio of the ingredients is adjusted to balance the heating time and the holding time, so as to avoid material splashing due to excessive heating or low conversion rate due to insufficient holding.

[0059] Step 5: Intelligent determination of process endpoint: Continuous monitoring When this value is less than a set minimum threshold for 5 consecutive sampling periods (e.g. ),and When the pressure stops rising, it indicates that the partial pressure of the inert gas can be migrated to atmospheric pressure throughout the process. The controller determines that the process has reached its end point and automatically performs cooling (starting and stopping the cooling fan cavity), shutting off heating, slowly backfilling inert gas to atmospheric pressure, and opening the baffle to transfer the product through multi-stage vacuum to the glove box chamber 200.

[0060] The working principle of this application is as follows: The glove box 200 is the core cavity for anaerobic inert operation. The external purification circulation device continuously maintains the stable atmosphere inside the chamber. The blower 300 relies on multiple sets of built-in purification columns in conjunction with the airflow circulation of the blower to continuously adsorb water vapor, oxygen and organic impurities inside the glove box 200. At the same time, the multiple sets of purification columns can alternately complete purification and regeneration operations to achieve uninterrupted atmosphere purification, stabilize the inert gas environment inside the chamber and reduce the overall purification load of the box. Meanwhile, the glove box 200 achieves seamless vacuum sealing docking with the multi-temperature zone RTP sublimation reaction unit through the transition transfer component. The high-temperature resistant vacuum sealing ring embedded in the inner side of the connecting flange 201 seals the docking gap and prevents air from entering the reaction structure from the docking gap. At the same time, the furnace body 100 encloses and forms a sealed heat-insulating cavity. The inner wall of the heat-insulating cavity is lined with nano heat-insulating cotton, which can isolate the heat interference between different heating areas and ensure the independent heating of each area. The glove box 200 is equipped with a graded independent vacuum material transfer unit. It adopts a partitioned independent compartment structure to realize the oxygen-free transfer of materials by category, completely avoiding the problems of air backflow and atmosphere pollution caused by sharing the transfer channel for materials of different specifications. Furthermore, the transfer compartment is equipped with independent feeding buffer compartment 207, small part rapid transfer compartment 206, and large part conveying transfer compartment 205, which do not interfere with each other. The three types of transfer compartments are independently equipped with vacuum pumping components, inert gas replenishment components and sealed opening and closing doors, so that the operation of each compartment does not interfere with each other. The feeding buffer chamber 207 completes the sealed feeding operation of materials by relying on the built-in automatic lifting feeding component 208, and the large-item conveying and transfer chamber 205 completes the stable transfer of large-sized materials by relying on the material conveying and supporting component. When a single set of transfer chambers is opened and closed, only the chamber itself is vacuumed and inert gas is replaced, which will not damage the inert vacuum environment of the main body of the glove box chamber 200. Materials of different specifications can be independently transferred to the transition transfer part as needed, and wait to be transferred to the multi-temperature zone RTP sublimation reaction chamber. Meanwhile, two interconnected operating chambers 203 are set inside the glove box 200. Operators can use the glove operating port 202 on the outside of the chamber to cooperate with the roller 204 at the bottom of the operating chamber 203 to support the material and complete auxiliary manual operations such as material arrangement, alignment and maintenance in the chamber without damaging the sealed and inert environment of the chamber. The vacuum unit is connected to the multi-temperature zone RTP sublimation reaction unit through a dedicated pipeline. The vacuum unit is controlled by the built-in vacuum pressure acquisition module of the controller 104. Before and during operation, the vacuum unit can independently evacuate the entire interior of the reaction tube 101 to match the negative pressure working environment required for material sublimation, further locking the vacuum seal inside the reaction tube 101 and preventing external air from seeping into the reaction area. After the material is sealed and transferred to the high-purity quartz reaction tube 101 via the transition transfer component, multiple independently arranged rapid heat treatment heating modules are activated to carry out the sublimation operation. Each group of rapid heat treatment heating modules is arranged along the axial direction of the reaction tube 101 and is independent of each other. The heating source is selected as an infrared lamp array or a laser heating source. Each group of heating modules can receive instructions from the independent temperature control module of the controller 104 and individually adjust the heating temperature of the corresponding reaction tube 101 section to achieve axial zone gradient heating of the reaction tube 101, which is suitable for the material segmented differentiated sublimation process requirements. A cooling fan 106 is installed between two adjacent rapid heat treatment heating modules. The fan is controlled by the controller 104 to start and stop, and can force heat dissipation in a local area of ​​the furnace body 100 to quickly regulate the local cavity temperature. An observation window 105 is provided on the side of the furnace body 100 to directly observe the sublimation state of the material inside the reaction tube 101. At the same time, the inner wall of the reaction tube 101 is sprayed with a high-temperature resistant and anti-adhesion coating to prevent the sublimated material from sticking to the tube wall, which facilitates material cleaning and tube wall maintenance after operation. Combined with the zoned temperature insulation of the nano heat insulation cotton inside the furnace body 100, the heat coupling interference between adjacent heating areas is completely eliminated, and the temperature control accuracy of a single tube section is accurately guaranteed. The device is equipped with an independent controller 104, which is electrically connected to the vacuum unit, all rapid heat treatment heating modules, graded independent vacuum material transfer components, purification circulation components, and cooling fan 106. At the same time, an external indicator light 103 provides visual prompts of the operating status. The controller 104 has a built-in independent temperature control module, vacuum pressure acquisition module, and timing linkage control module, which can uniformly control the operating parameters of the entire device. It automatically matches the vacuum degree of the cavity, the start and stop of zone heating and heating temperature, the start and stop sequence of material transfer, the start and stop of chamber purification, and the start and stop of fan cooling at each stage. The timing linkage matches the entire process of material feeding, vacuum replacement, sealed transfer, zone gradient sublimation, cavity depressurization, finished product return, and atmosphere purification. No manual operation is required at each step. The closed loop realizes the fully automated linkage operation of the entire process of oxygen-free vacuum transfer of materials, zone gradient heating and sublimation, and device atmosphere purification. In case of abnormal operating conditions of the device, the indicator light 103 will light up simultaneously to prompt the operation and maintenance personnel to handle the situation. Taking molybdenum dioxide (MoO2Cl2) as an example, take 0-10 kg (e.g., 500 g) of 99.5% pure molybdenum dioxide raw material and place it in a quartz boat. Place the boat in the middle of reaction tube 101, close the gate valve in connecting flange 201, and start the vacuum unit to evacuate the pressure inside reaction tube 101 to ≤5×10⁻⁶. -2 mbar; The system is set up with four temperature zones: the first temperature zone is a preheating zone heated to 130±5℃, the second temperature zone is a sublimation zone heated to 300-400℃, the third temperature zone is a cooling zone cooled to 180±5℃, and the fourth temperature zone is a collection zone kept naturally cooled to 80±5℃. The heating rate is about 50℃ / min, and the holding time is 60 minutes. After sublimation, high-purity argon gas is slowly backfilled to atmospheric pressure. The collected product is then removed through the glove box by opening the gate valve. For other Mo-type precursors, the temperature and holding time of each temperature zone can be adjusted according to their physical properties (such as sublimation temperature, vapor pressure curve, etc.). This system is also applicable.

[0061] The above are merely preferred embodiments of the present invention and are not intended to limit the implementation methods and protection scope of the present invention. Those skilled in the art should recognize that any equivalent substitutions and obvious changes made based on the description and illustrations of the present invention should be included within the protection scope of the present invention.

Claims

1. A glove box multi-temperature zone RTP sublimation purification integrated system, comprising a glove box chamber (200) and a vacuum unit, characterized in that, It also includes a multi-zone RTP sublimation reactor, which is sealed to the glove box (200) via a transition transfer member; the vacuum unit is connected to the multi-zone RTP sublimation reactor via a pipeline for evacuating the multi-zone RTP sublimation reactor; the multi-zone RTP sublimation reactor includes a furnace body (100) and a reaction tube (101), as well as multiple sets of independently arranged rapid heat treatment heating modules arranged axially along the reaction tube (101), each set of rapid heat treatment heating modules is fixedly connected to the top of the furnace body (100), and each rapid heat treatment heating module can independently control and heat the corresponding section of the reaction tube (101).

2. The integrated multi-temperature zone RTP sublimation purification system for glove boxes according to claim 1, characterized in that, The glove box (200) is equipped with a graded independent vacuum material transfer device inside. The graded independent vacuum material transfer device is used to classify and isolate the transfer of materials, avoid the intrusion of outside air into the glove box (200) caused by the sharing of channels for materials of different specifications, stabilize the inert atmosphere inside the glove box (200), and reduce the purification load of the box. A purification circulation device is provided on one side of the external side of the glove box (200) for alternating purification and regeneration and continuous adsorption of water vapor, oxygen and organic impurities in the box.

3. The integrated multi-temperature zone RTP sublimation purification system for glove boxes according to claim 1, characterized in that, The rapid heat treatment heating module includes an infrared lamp array or a laser heating source.

4. The integrated multi-temperature zone RTP sublimation purification system for glove boxes according to claim 3, characterized in that, A forced cooling fan (106) is provided on the surface of the furnace body (100) and between two adjacent sets of rapid heat treatment heating modules. An observation window (105) is provided on the surface of the furnace body (100) and on one side of the cooling fan (106).

5. The integrated multi-temperature zone RTP sublimation purification system for glove boxes according to claim 1, characterized in that, The glove box (200) has two interconnected operating chambers (203) on one side. The bottom of the operating chamber (203) is provided with multiple sets of rollers (204) for supporting materials. The surface of the glove box (200) and the position of each set of operating chambers (203) are provided with glove operating openings (202).

6. The integrated multi-temperature zone RTP sublimation purification system for glove boxes according to claim 2, characterized in that, The graded independent vacuum material transfer unit includes a feeding buffer chamber (207), a small part rapid transfer chamber (206), and a large part conveying transfer chamber (205) located inside the other side of the glove box (200) and divided into non-interfering feeding buffer chamber (207), small part rapid transfer chamber (206), and large part conveying transfer chamber (205). The feeding buffer chamber (207) has an automatic lifting feeding component (208) built in, and the large part conveying transfer chamber (205) has a material conveying support component built in. The feeding buffer chamber (207), small part rapid transfer chamber (206), and large part conveying transfer chamber (205) are each independently equipped with a vacuum pumping component, an inert gas replenishment component, and a sealed opening and closing door.

7. The integrated multi-temperature zone RTP sublimation purification system for glove boxes according to claim 2, characterized in that, The purification circulation component includes a fan barrel (300) disposed outside the glove box (200). The fan barrel (300) is provided with multiple sets of purification columns inside. The fan barrel (300) is connected to the inside of the glove box (200) through a connecting pipe (302).

8. The integrated multi-temperature zone RTP sublimation purification system for glove boxes according to claim 7, characterized in that, The transition transfer component includes a connecting flange (201) disposed on one side of the glove box (200). The other end of the connecting flange (201) is connected to the furnace body (100), and a high-temperature vacuum sealing ring is embedded inside the connecting flange (201) to achieve seamless vacuum sealing docking between the glove box (200) and the furnace body (100). A high-vacuum gate valve or gate valve is integrated inside the connecting flange (201) for closing after the material transfer is completed, so that the reaction tube (101) and the glove box (200) are airtightly isolated.

9. The integrated multi-temperature zone RTP sublimation purification system for glove boxes according to claim 1, characterized in that, The reaction tube (101) is made of high-purity quartz material. The inner wall of the reaction tube (101) is sprayed with a high-temperature resistant and anti-adhesion coating. The furnace body (100) is enclosed to form a sealed heat-insulating cavity. The inner wall of the heat-insulating cavity is lined with nano heat-insulating cotton to isolate the heat from each group of rapid heat treatment heating modules and ensure the temperature control accuracy of a single tube section.

10. The integrated multi-temperature zone RTP sublimation purification system for glove boxes according to claim 1, characterized in that, It also includes a controller (104) and an indicator light (103) electrically connected to the signal output terminal of the controller (104). The controller (104) is electrically connected to a vacuum unit, multiple sets of rapid heat treatment heating modules, graded independent vacuum material transfer components, purification circulation components, and a cooling fan (106). The controller (104) has a built-in independent temperature control module, a vacuum pressure acquisition module, and a timing linkage control module, which are used to uniformly regulate the vacuum degree of the device, the zone heating temperature, the material transfer sequence, and the start and stop of the box purification, so as to realize the full-process automated linkage operation of oxygen-free vacuum transfer of materials, zoned gradient heating and sublimation, and device atmosphere purification.

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