Method for safe filling of diborane mixtures

Abstract

This invention discloses a safe filling method for diborane mixed gas. This invention relates to the field of gas filling technology. It utilizes dual sensing units to collect the concentration of diborane decomposition byproducts in real time, and employs a closed-loop control algorithm to correlate and dynamically correct filling pressure, flow rate, and temperature. Combined with comprehensive safety management throughout the entire process, it addresses the risk of hidden decomposition. The advantages of this invention are: real-time capture of diborane decomposition byproduct concentration through dual sensing units; establishing and dynamically correcting the correlation between byproduct concentration and filling pressure, flow rate, and temperature using a closed-loop control algorithm; and comprehensive management including pre-treatment of gas cylinders before filling and harmless treatment of residual gas in pipelines after filling. This solves the core defects of existing technologies, such as the lack of a linkage mechanism between byproducts and filling parameters and the inability to identify hidden decomposition risks.

Description

Technical Field

[0001] This invention relates to the field of gas filling technology, specifically a safe filling method for a mixture of borane and diethylborane. Background Technology

[0002] Diborane mixtures, as industrial gases with special application value, are widely used in high-end fields such as semiconductor manufacturing, chemical synthesis, materials science, and aerospace. In the semiconductor industry, diborane mixtures are often used as doping sources in the p-type doping process of silicon wafers. Their purity and concentration stability directly affect the electrical performance and yield of semiconductor devices. In the field of chemical synthesis, this mixture can be used as a catalyst or reaction intermediate to participate in the synthesis reaction of specific organic compounds, promoting the preparation of high-value-added chemical products. In the field of materials science, diborane mixtures can also be used to prepare high-performance boride ceramic materials, providing key support for material surface modification and performance optimization.

[0003] Existing borane mixed gas filling operations mainly rely on preset fixed filling pressures, flow rates, and basic cylinder cleaning procedures to achieve gas injection. This approach has certain shortcomings. First, it lacks a linkage mechanism between borane decomposition byproducts and filling parameters, making it impossible to detect the "hidden decomposition risk of parameters meeting standards but byproducts exceeding standards." Furthermore, it lacks comprehensive safety control measures. Second, it lacks a data traceability system for the entire filling process, making it impossible to trace the source of quality problems. There are also no targeted post-filling leakage detection and quality verification procedures. Therefore, we propose a safe filling method for borane mixed gas. Summary of the Invention

[0004] The purpose of this invention is to provide a safe filling method for ethylene borane mixed gas.

[0005] To achieve the above objectives, the present invention provides the following technical solution: a safe filling method for a borane mixture, the safe filling method comprising the following steps:

[0006] Step 1: Select suitable gas filling equipment and perform container pretreatment on the filling gas cylinders, and establish a safety threshold library for diborane decomposition byproducts. The container pretreatment includes inert gas purging-vacuuming operation.

[0007] Step 2: Pre-charge the gas cylinder with low-pressure gas at a preset low pressure and low flow rate, monitor the concentration of borane decomposition byproducts in real time during the pre-charging process, and proceed to the main charging stage after confirming that there is no risk of decomposition.

[0008] Step 3: Start the main filling program to fill the gas cylinder with a mixture of diborane and hydrogen. The concentration of decomposition byproducts (hydrogen and boron oxides) is collected in real time using a dual-sensor unit. A closed-loop control algorithm is used to dynamically adjust the gas filling parameters (pressure, flow rate, and temperature). The adjustment formula for the closed-loop control algorithm is as follows:

[0009] ;

[0010] ;

[0011] ;

[0012] in, Real-time gas filling pressure (unit: MPa). Initial filling pressure (unit: MPa). The coefficient representing the influence of hydrogen concentration. This is a pressure correction factor;

[0013] Real-time gas filling flow rate (unit: m / s). Initial filling flow rate of the main filler (unit: m / s). The coefficient representing the influence of boron oxide concentration is... This is a flow rate correction factor;

[0014] Real-time gas filling control temperature (unit: °C). Main charge initial control temperature (unit: °C). This is a temperature correction factor. Temperature co-factor;

[0015] Hydrogen concentration (unit: ppm). boron oxide concentration (unit: mg / m³) 3 );

[0016] Step 4: When the main filling reaches 90%-95% of the target total filling volume, switch to the supplementary gas filling mode, and gradually reduce the filling pressure and flow rate until the mixed gas reaches the target total filling volume.

[0017] Step 5: After closing the gas cylinder valve, perform residual gas recovery and harmless treatment on the gas filling pipeline.

[0018] As a further aspect of the present invention: the piping material of the gas filling equipment is Hastelloy C-276, the sealing element is made of perfluoroelastomer, and the gas filling system is equipped with a hydrogen trace sensor (detection limit ≤ 1 ppm) and a boron oxide optical sensor (detection accuracy ≤ 0.1 mg / m³). 3The container pretreatment involves three cycles of inert gas purging and vacuuming. Each purging cycle uses an inert gas pressure of 0.4-0.6 MPa and a purging time of 30-60 seconds. Vacuuming is performed until the container's pre-vacuum level is ≤1 Pa, ensuring that residual moisture in the gas cylinder is ≤5 ppm and oxygen is ≤3 ppm. The safety threshold library for diborane decomposition byproducts is set with a hydrogen safety warning threshold of 5 ppm, an emergency shutdown threshold of 10 ppm, and a boron oxide deposition warning threshold of 0.3 mg / m³. 3 Emergency shutdown threshold: 0.5 mg / m³ 3 At the same time, input the preset filling concentration of the gas mixture (0.1%-10%) and the nominal volume of the gas cylinder (40-100L) as basic parameters.

[0019] As a further aspect of the present invention: In step two, the pre-filling pressure of the low-pressure gas is 0.3 MPa, the filling flow rate is ≤1 m / s, the pre-filling amount is 5%-8% of the target total filling amount, the gas filling environment temperature during the pre-filling stage is controlled at 10℃-15℃, and the filling pressure fluctuation throughout the process is ≤±0.05 MPa. If hydrogen concentration is detected... ≥5ppm, boron oxide concentration ≥0.3mg / m 3 If any of these conditions are met, immediately stop the gas pre-charging, start the inert gas purging (purging pressure 0.5MPa, purging time 60s) - vacuuming (vacuum degree ≤1Pa) cycle once, and then restart the low-pressure gas pre-charging.

[0020] As a further aspect of the present invention: In step three, the initial gas filling pressure of the main filling process is 0.8MPa-1.2MPa, the initial gas filling flow rate is 1.5m / s-2.0m / s, the gas filling ambient temperature during the main filling stage is maintained at 10℃-20℃, and the dual sensing unit collects decomposition byproduct concentration data every 2s-3s. The value is 0.08 ppm. -1 -0.12ppm -1 , The value ranges from 0.8 to 1.0. The value is 0.3-0.5mg. -1 ·m 3 , The value ranges from 0.7 to 0.9. Take the value at 2℃·mg -1 ·m 3 -3℃·mg -1 ·m 3 , The hydrogen concentration is controlled throughout the main charging phase, with a value ranging from 0.9 to 1.1. <8ppm, boron oxide concentration <0.4mg / m 3If any parameter reaches the emergency shutdown threshold, the gas filling circuit will be immediately cut off and the inert gas isolation protection will be activated. The main filling will continue until the borane mixture reaches 90%-95% of the target total filling volume.

[0021] As a further aspect of the present invention: In step four, the filling pressure gradient of the supplementary gas filling is ≤0.1MPa per 10s, the initial filling flow rate is reduced to 0.8m / s-1.0m / s, the mixed gas concentration is monitored in real time by a sensing unit, and when the concentration reaches ±0.1% of the preset filling concentration, the gas filling pressure is gradually reduced to 0.5MPa, the filling flow rate is maintained at 0.5m / s and filling continues until the target total filling volume is reached, and the hydrogen concentration is monitored throughout the filling stage. ≤5ppm, boron oxide concentration ≤0.3mg / m 3 If parameter fluctuations occur, they are synchronously corrected using the closed-loop formula for gas filling parameters in step three.

[0022] As a further aspect of the present invention: In step five, the residual gas recovery and harmless treatment involves purging with inert dilution gas followed by vacuuming 2-3 times, with each purging cycle consisting of a pressure of 0.3MPa-0.4MPa and a purging time of 45s-60s, followed by vacuuming to a vacuum degree ≤1Pa. After treatment, the hydrogen concentration at the pipeline outlet is measured to be ≤0.5ppm and the boron oxide concentration to be ≤0.05mg / m³. 3 The residual gas is converted into non-toxic borate and water vapor by a catalytic decomposition device before being discharged.

[0023] As a further aspect of the present invention: the safe filling method further includes step six, which involves using a combination of laser spectroscopy leak detection and pressure attenuation method to detect leaks in the filled gas cylinder and verify the filling quality of the borane mixture.

[0024] Leak detection was performed using laser spectroscopy (detection sensitivity ≤ 1×10⁻⁶). -6 Pa·m 3 The method combines pressure decay (≤0.02MPa within 12 hours) with the pressure decay method. Detection sites include cylinder valves, interfaces, and filling connectors. Mixed gas quality verification uses gas chromatography to detect diborane concentration (deviation ≤±0.2%), and sensor methods to detect hydrogen concentration ≤3ppm and boron oxide concentration ≤0.1mg / m³. 3 Ensure that the purity of the mixed gas is ≥99.99%.

[0025] As a further aspect of the present invention: the safe filling method further includes step seven, which is to record key parameters of the entire gas filling process and establish a traceable management system for the filling process.

[0026] Key parameters recorded throughout the gas filling process include: gas filling equipment model and material information, cylinder pretreatment parameters (purge pressure / time, vacuum degree), decomposition byproduct threshold database data, real-time filling parameters (pressure / flow rate / temperature) and correction records for each stage of pre-filling / main filling / replenishment, parameters for the harmless treatment of residual gas recovery in filling pipelines, cylinder leakage detection results, and mixed gas filling quality inspection data. All parameter data are stored on an encrypted server with a data retention period of ≥5 years. The entire process can be traced using the unique cylinder number and gas filling date, with a traceability response time of ≤10 minutes.

[0027] Compared with the prior art, the beneficial effects of the present invention by adopting the above technical solution are as follows:

[0028] 1. This invention uses dual sensing units to capture the concentration of decomposition byproducts of borane in real time. By employing a closed-loop control algorithm, it establishes a correlation between the byproduct concentration and filling pressure, flow rate, and temperature, and dynamically corrects the correlation. Combined with full-process control, including pre-treatment of gas cylinders before filling and harmless treatment of residual gas in pipelines after filling, this invention solves the core defects of existing technologies, such as the lack of a linkage mechanism between byproducts and filling parameters and the inability to identify hidden decomposition risks. This mechanism can detect the "hidden problem of parameters meeting the standards but byproducts exceeding the standards" in real time, effectively suppressing the accumulation of byproducts and reducing safety hazards. At the same time, it suppresses the decomposition chain reaction from the source to ensure the stability of the mixed gas composition, ultimately achieving the technical effect of safe and controllable filling process of borane mixed gas with reliable quality.

[0029] 2. This invention addresses the shortcomings of existing technologies by constructing a parameter traceability management system for the entire filling process of borane mixed gas, coupled with targeted leak detection and quality verification after filling. This system solves the problems of existing technologies, such as the lack of data retention during the filling process, the inability to trace the source of quality problems, and the difficulty in ensuring subsequent safety. The system can completely record key information at each filling stage, providing accurate traceability for potential quality or safety issues. The quality verification process further filters out unqualified products, preventing them from entering the usage stage. Ultimately, this invention improves the efficiency of problem identification and subsequent safety during the filling process of borane mixed gas, and helps to achieve full life-cycle control of filling. Attached Figure Description

[0030] Figure 1 This is a schematic diagram of the method steps in an embodiment of the present invention;

[0031] Figure 2 This is a schematic diagram of the process for monitoring decomposition byproducts and controlling parameters in the main charging stage, as described in an embodiment of the present invention. Detailed Implementation

[0032] The specific embodiments of the present invention will be further described below with reference to the accompanying drawings. It should be noted that the description of these embodiments is for the purpose of helping to understand the present invention, but does not constitute a limitation of the present invention.

[0033] Furthermore, the technical features involved in the various embodiments of the present invention described below can be combined with each other as long as they do not conflict with each other.

[0034] Please see the appendix Figure 1 -Appendix Figure 2 The present invention discloses a safe filling method for a mixture of diborane and ethylene, comprising the following steps:

[0035] Step 1: Select suitable gas filling equipment and pre-treat the filling cylinders. Establish a safety threshold library for diborane decomposition byproducts. Container pre-treatment includes inert gas purging and vacuuming.

[0036] Step 2: Pre-charge the gas cylinder with low-pressure gas at a preset low pressure and low flow rate, monitor the concentration of borane decomposition byproducts in real time during the pre-charging process, and proceed to the main charging stage after confirming that there is no risk of decomposition.

[0037] Step 3: Start the main filling program to fill the gas cylinder with a mixture of diborane and hydrogen. The concentration of decomposition byproducts (hydrogen and boron oxides) is collected in real time using a dual-sensor unit. A closed-loop control algorithm is used to dynamically adjust the gas filling parameters (pressure, flow rate, and temperature). The adjustment formula for the closed-loop control algorithm is as follows:

[0038] ;

[0039] ;

[0040] ;

[0041] in, Real-time gas filling pressure (unit: MPa). Initial filling pressure (unit: MPa). The coefficient representing the influence of hydrogen concentration. This is a pressure correction factor;

[0042] Real-time gas filling flow rate (unit: m / s). Initial filling flow rate of the main filler (unit: m / s). The coefficient representing the influence of boron oxide concentration is... This is a flow rate correction factor;

[0043] Real-time gas filling control temperature (unit: °C). Main charge initial control temperature (unit: °C). This is a temperature correction factor. Temperature co-factor;

[0044] Hydrogen concentration (unit: ppm). boron oxide concentration (unit: mg / m³) 3 );

[0045] coefficient , , , , , The value range is pre-calibrated based on a large amount of experimental data and the decomposition kinetic model of diborane, and stored in the control system;

[0046] Step 4: When the main filling reaches 90%-95% of the target total filling volume, switch to the supplementary gas filling mode, and gradually reduce the filling pressure and flow rate until the mixed gas reaches the target total filling volume.

[0047] Step 5: After closing the gas cylinder valve, perform residual gas recovery and harmless treatment on the gas filling pipeline.

[0048] Example 1, please refer to the appendix. Figure 1 -Appendix Figure 2 The closed-loop control algorithm further illustrates its operation process in actual filling. When filling a mixture with a nominal volume of 60L and a preset diborane concentration of 5%, the initial main filling pressure is set to 1.0MPa, the initial flow rate to 1.8m / s, and the initial temperature to 15℃. The dual-sensor unit collects data every 2 seconds. When the hydrogen concentration is detected to rise to 6ppm (not reaching the warning threshold but showing an upward trend), the system automatically substitutes the closed-loop formula: real-time filling pressure... =1.0×(1-0.1×6×0.9)=0.46MPa, real-time flow rate =1.8×(1-0.4×0.2×0.8)=1.6848m / s, real-time temperature =15-2.5×(0.1×6+0.4×0.2)×1.0=13.3℃. By dynamically adjusting the parameters, the hydrogen concentration gradually decreased to 3ppm, effectively inhibiting further decomposition of diborane and ensuring the stability of the main charging process.

[0049] Example 2, please refer to the appendix. Figure 1 -Appendix Figure 2For the pretreatment of gas cylinders, specific operational details are supplemented. After selecting the gas cylinder to be filled, argon gas, which is consistent with the dilution gas of the mixed gas, is first used as the purging gas. During the first purging, the argon gas pressure is stabilized to 0.5 MPa and continuously introduced for 45 seconds. Then, the vacuum pump is started to evacuate to a vacuum degree of 0.8 Pa and the vacuum state is maintained for 30 seconds to ensure that the residual gas is fully discharged. The above purging-vacuuming process is repeated 3 times. The pressure fluctuation of each purging is controlled within ±0.03 MPa. After the third cycle, the residual moisture in the gas cylinder is detected by a gas analyzer to be 3 ppm and the oxygen is 2 ppm, which meets the pretreatment requirements and avoids the safety risks caused by the reaction of residual impurities with diborane.

[0050] Example 3, please refer to the appendix. Figure 1 -Appendix Figure 2 The residual gas recovery and harmless treatment process involves specific operational steps. After refilling and closing the cylinder valve, inert dilution gas (nitrogen) is first introduced into the filling pipeline to raise the pressure to 0.35 MPa and maintain this pressure for 50 seconds. The nitrogen then propels the residual diborane mixture in the pipeline towards the residual gas recovery and harmless treatment device. Subsequently, a vacuum pump is started to evacuate the pipeline to 0.9 Pa, completing the first purging-vacuuming cycle. This cycle is repeated twice. Afterward, the sensor at the pipeline outlet detects a hydrogen concentration of 0.3 ppm and a boron oxide concentration of 0.03 mg / m³. 3 The residual gas is converted into borate and water vapor by a catalytic decomposition device before being discharged, thus avoiding residual gas leakage, pollution, or safety accidents.

[0051] Specifically, the dual-sensor unit is implemented as follows: a hydrogen micro-sensor is installed in the filling pipeline near the gas cylinder interface (15cm from the interface), and a boron oxide optical sensor is installed in the middle section of the pipeline (1m from the sensor). Both are connected to the filling control system via wired connection, with a data transmission delay of ≤0.5s. When either sensor detects an abnormal data, it immediately sends a signal to the control system, which synchronously triggers a parameter correction command to ensure the coordination of data acquisition and parameter control between the two sensors, avoiding control lag caused by a single sensor failure or data abnormality.

[0052] Specifically, the multi-dimensional leak detection is implemented as follows: First, a laser spectral leak detector is used to scan and detect the sealing surfaces of the gas cylinder valve interface and filling connector. During the detection, the leak detector probe is placed close to the detection area, and the moving speed is controlled at 5cm / s. Each sealing surface is scanned twice. After the laser detection shows no abnormalities, the pressure decay method is used to stabilize the gas cylinder pressure at 1.2MPa. The initial pressure is recorded and then left to stand for 12 hours. The pressure is recorded every 2 hours during this period. After 12 hours, the pressure decay is 0.015MPa, which meets the requirement of ≤0.02MPa. Through the combination of "precisely locating micro-leakage first and then verifying the overall sealing performance", leakage risks are comprehensively investigated.

[0053] Specifically, the full-process data traceability is implemented as follows: data acquisition nodes are set up at the pressure sensor, flow controller, temperature sensor, and dual-sensor unit of the filling equipment to collect parameters at each stage in real time and automatically associate them with the unique cylinder number and filling date. The collected data is uploaded to the cloud encrypted server through an encrypted transmission protocol. The server is set with hierarchical permissions (operators can only view, administrators can export). When it is necessary to trace a cylinder of mixed gas, the cylinder number can be entered to retrieve the full-process data from pretreatment to quality verification within 10 minutes, so that problems can be found and responsibilities can be traced.

[0054] Working principle:

[0055] First, suitable gas filling equipment is selected, and the filling cylinders undergo inert gas purging and vacuum pretreatment. Simultaneously, a safety threshold database for diborane decomposition byproducts is established to eliminate the risk of impurities in the cylinders reacting with diborane. Next, the cylinders are pre-filled at low pressure and low flow rate, with real-time monitoring of the decomposition byproduct concentration. Once no decomposition risk is confirmed, the main filling stage begins. During main filling, hydrogen and boron oxide concentrations are collected in real-time using dual-sensor units. A closed-loop control algorithm links the byproduct concentration with filling pressure, flow rate, and temperature, dynamically adjusting parameters to suppress diborane decomposition. When the main filling reaches 90%-95% of the target total filling volume, the system switches to supplementary filling mode, fine-tuning parameters to achieve the target total filling volume. The cylinder valve is then closed, and residual gas in the filling pipeline is recovered and rendered harmless to prevent leakage. Cylinder leaks are detected using a combination of laser spectroscopy and pressure attenuation methods, and the mixed gas quality is verified. Finally, key parameters throughout the entire process are recorded, and a traceability system is established for subsequent troubleshooting. This concludes the entire workflow.

[0056] Although the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make possible changes and modifications without departing from the spirit and scope of the present invention. Therefore, any modifications, equivalent changes and alterations made to the above embodiments based on the technical essence of the present invention without departing from the content of the technical solution of the present invention shall fall within the protection scope defined by the claims of the present invention.

Claims

1. A safe filling method for a mixture of diborane gas, characterized in that, The safe filling method includes the following steps: Step 1: Select suitable gas filling equipment and pre-treat the filling cylinders to establish a safety threshold library for diborane decomposition byproducts. Step 2: Pre-charge the gas cylinder with low-pressure gas at a preset low pressure and low flow rate, monitor the concentration of borane decomposition byproducts in real time during the pre-charging process, and proceed to the main charging stage after confirming that there is no risk of decomposition. Step 3: Start the main filling program to fill the gas cylinder with a mixture of diborane and borane. The concentration of decomposition byproducts is collected in real time using a dual-sensor unit. A closed-loop control algorithm is used to dynamically correct the gas filling parameters. The correction formula for the closed-loop control algorithm is as follows: ； ； ； in, For real-time gas filling pressure, The initial charge pressure for the main charge. The coefficient representing the influence of hydrogen concentration. This is a pressure correction factor; For real-time gas filling flow rate, The initial charge flow rate for the main charge. The coefficient representing the influence of boron oxide concentration is... This is a flow rate correction factor; To control the gas filling temperature in real time, Main charge initial control temperature This is a temperature correction factor. Temperature co-factor; Hydrogen concentration, This refers to the concentration of boron oxides. Step 4: When the main filling reaches 90%-95% of the target total filling volume, switch to the supplementary gas filling mode, and gradually reduce the filling pressure and flow rate until the mixed gas reaches the target total filling volume. Step 5: After closing the gas cylinder valve, perform residual gas recovery and harmless treatment on the gas filling pipeline.

2. The safe filling method for a borane mixture according to claim 1, characterized in that: In step one, the piping material of the gas filling equipment is Hastelloy C-276, the seals are made of perfluoroelastomer, the gas filling system is equipped with a hydrogen trace sensor and a boron oxide optical sensor, the container pretreatment uses three inert gas purging-vacuum cycles, and the safety threshold library for diborane decomposition byproducts is set with a hydrogen safety warning threshold of 5 ppm, an emergency shutdown threshold of 10 ppm, and a boron oxide deposition warning threshold of 0.3 mg / m³. 3 Emergency shutdown threshold: 0.5 mg / m³ 3 At the same time, input the preset filling concentration of the mixed gas and the basic parameters of the nominal volume of the gas cylinder.

3. The safe filling method for a borane mixture according to claim 2, characterized in that: In step two, the pre-filling pressure of the low-pressure gas is 0.3 MPa, the filling flow rate is ≤1 m / s, and the pre-filling amount is 5%-8% of the target total filling amount. During the pre-filling stage, the ambient temperature is controlled at 10℃-15℃, and the total filling pressure fluctuation is ≤±0.05 MPa. If hydrogen concentration is detected... ≥5ppm, boron oxide concentration ≥0.3mg / m 3 If any of these conditions are met, immediately suspend the gas pre-charge, initiate one inert gas purging-vacuuming cycle, and then restart the low-pressure gas pre-charge.

4. The safe filling method for a borane mixture according to claim 3, characterized in that: In step three, the dual-sensor unit collects decomposition byproduct concentration data every 2-3 seconds. The value is 0.08 ppm. -1 -0.12ppm -1 , The value ranges from 0.8 to 1.

0. The value is 0.3-0.5mg. -1 ·m 3 , The value ranges from 0.7 to 0.

9. Take the value at 2℃·mg -1 ·m 3 -3℃·mg -1 ·m 3 , The hydrogen concentration is controlled throughout the main charging phase, with a value ranging from 0.9 to 1.

1. <8ppm, boron oxide concentration <0.4mg / m 3 If any parameter reaches the emergency shutdown threshold, the gas filling circuit will be immediately cut off and the inert gas isolation protection will be activated. The main filling will continue until the borane mixture reaches 90%-95% of the target total filling volume.

5. The safe filling method for a borane mixture according to claim 4, characterized in that: In step four, the filling pressure gradient for supplementary gas filling is ≤0.1MPa increase every 10s. The initial filling flow rate is reduced to 0.8m / s-1.0m / s. The gas mixture concentration is monitored in real time by a sensing unit. When the concentration reaches ±0.1% of the preset filling concentration, the gas filling pressure is gradually reduced to 0.5MPa, and the filling flow rate is maintained at 0.5m / s to continue filling until the target total filling volume is reached. The hydrogen concentration is monitored throughout the filling phase. ≤5ppm, boron oxide concentration ≤0.3mg / m 3 If parameter fluctuations occur, they are synchronously corrected using the closed-loop formula for gas filling parameters in step three.

6. The method for safe filling of a borane mixture according to claim 5, characterized in that: In step five, the residual gas recovery and harmless treatment involves purging with inert dilution gas followed by vacuuming 2-3 times. Each purging cycle has a pressure of 0.3-0.4 MPa and a duration of 45-60 seconds. Vacuuming is then performed until the vacuum level is ≤1 Pa. After treatment, the hydrogen concentration at the pipeline outlet is measured to be ≤0.5 ppm and the boron oxide concentration to be ≤0.05 mg / m³. 3 The residual gas is converted into non-toxic borate and water vapor by a catalytic decomposition device before being discharged.

7. The safe filling method for a borane mixture according to claim 6, characterized in that: The safe filling method also includes step six, which involves using a combination of laser spectroscopy leak detection and pressure attenuation method to detect leaks in the filled gas cylinder and verify the filling quality of the borane mixture.

8. The safe filling method for a borane mixture according to claim 7, characterized in that: The safe filling method also includes step seven, which involves recording key parameters of the entire gas filling process and establishing a traceable management system for the filling process.

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