A silane mixed gas composite nanocatalysis-temperature sensitive intelligent control system and efficient stirring process
Through the intelligent control system of nano-tungsten carbide and graphene quantum dot composite catalyst and temperature-sensitive polymer gel microspheres, combined with electromagnetic synergistic technology, the problems of low mixing efficiency and poor safety of silane mixed gas are solved, and an efficient, stable and safe mixing effect is achieved.
Patent Information
- Application Number
- CN202510964236.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-14
- Publication Date
- 2025-09-26
- Estimated Expiration
- 2045-07-14
AI Technical Summary
The existing silane gas mixing process has problems such as low mixing efficiency, poor safety, and insufficient stability. Traditional surfactants and catalysts are difficult to meet the requirements of efficient mixing, and there is a lack of precise control means for the mixing process.
A composite nanocatalysis-temperature-sensitive intelligent control system consisting of nano-tungsten carbide and graphene quantum dot composite nanocatalysts, modified silicone surfactants and temperature-sensitive polymer gel microspheres is used, combined with an electric field-magnetic field synergistic device and microfluidic pretreatment technology to achieve efficient stirring and precise control.
It significantly improves mixing uniformity, shortens mixing time, reduces explosion risk, enhances storage stability, reduces energy consumption, and meets high-end application requirements.
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Figure CN120459866B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of micro-chemical engineering and process intensification, and specifically to a silane mixed gas composite nano-catalysis-temperature-sensitive intelligent control system and a high-efficiency stirring process. Background Art
[0002] Silane gas mixtures play an indispensable role in semiconductor manufacturing, the photovoltaic industry, and thin-film coating technology. In semiconductor integrated circuit manufacturing, silane gas mixtures are used in the chemical vapor deposition (CVD) process and are a key raw material for producing high-quality silicon-based thin films. Their mixing uniformity and stability directly impact the performance and yield of semiconductor devices. In the photovoltaic industry, silane gas mixtures are used to prepare key layers in silicon-based solar cells, and the quality of the mixture determines the cell's photovoltaic conversion efficiency. Furthermore, in optical coatings and nanomaterial preparation, the performance of silane gas mixtures also has a decisive impact on the quality of the final product.
[0003] However, existing silane gas mixing processes present numerous challenges. Traditional mechanical stirring methods rely solely on the rotation of paddles to achieve gas mixing, resulting in low mixing efficiency and difficulty achieving a fully uniform blend of silane and diluent gas in a short period of time. Due to silane's flammability, explosiveness, and chemically reactive properties, localized overconcentrations can easily occur during the mixing process, increasing the risk of explosion and leading to premature decomposition of silane, producing impurities such as silicon particles, which can affect the purity and stability of the gas mixture.
[0004] Conventional surfactants and catalysts struggle to meet the requirements for efficient mixing when it comes to additives in mixing systems. Ordinary surfactants have limited ability to emulsify and disperse gases, failing to effectively reduce gas-gas interfacial tension, leading to stratification of the mixed gas. Traditional catalysts often require high reaction temperatures and long reaction times to promote the decomposition and uniform distribution of silane, increasing energy consumption and potentially causing excessive decomposition of the silane, resulting in undesirable side effects.
[0005] Furthermore, existing mixing processes lack precise control over the mixing process. Even slight changes in environmental factors like temperature and pressure can significantly impact the mixing quality and stability of the silane mixture. For example, temperature fluctuations can alter the decomposition rate of silane, affecting the composition and performance of the mixture. Furthermore, static electricity generated during the mixing process can cause accidental combustion or explosion of silane, and current processes lack effective control measures.
[0006] As industries like semiconductors and photovoltaics move toward higher precision and reliability, the quality requirements for silane gas mixtures are becoming increasingly stringent. Traditional mixing processes are no longer able to meet these demands, and there is an urgent need to develop a new stirring and mixing process that can achieve efficient and uniform mixing while ensuring gas mixture stability and safety. This will drive technological upgrades and sustainable development in related industries. Summary of the Invention
[0007] (1) Technical problems solved
[0008] In response to the deficiencies of the prior art, the present invention provides a silane mixed gas composite nanocatalysis-temperature-sensitive intelligent control system and an efficient stirring process.
[0009] (2) Technical solution
[0010] A silane gas mixture composite nanocatalysis-temperature-sensitive intelligent control system comprises silane, a diluent gas, a nanocatalyst composed of nano-tungsten carbide and graphene quantum dots (GQDs), a modified organosilicon surfactant, and temperature-sensitive polymer gel microspheres as an intelligent control additive; the diluent gas is hydrogen, helium, or a mixture of the two; the nano-tungsten carbide accounts for 40-60% by weight of the composite nanomaterial, and the addition amount is 0.05-0.5% of the total mass of the mixed system; the volume fraction of silane in the mixed gas is 5-25%; the modified organosilicon surfactant is made of polydimethylsiloxane grafted with polyether groups and fluorocarbon chains, and the addition amount is 0.1-1%, the polyether group grafting rate is 15-30%, and the fluorocarbon chain grafting rate is 5-15%; the temperature-sensitive polymer gel microspheres use N-isopropylacrylamide as a monomer; the structural formula of the polydimethylsiloxane is:
[0011]
[0012] The structural formula of polyether group grafted polydimethylsiloxane is:
[0013]
[0014] The structural formula of fluorocarbon chain grafted polydimethylsiloxane is:
[0015]
[0016] The structural formula of the N-isopropylacrylamide is:
[0017]
[0018] Preferably, the nano-tungsten carbide particle size is 5-20 nanometers, the graphene quantum dot particle size is 2-10 nanometers, and both surfaces are amino treated, with an amino density of 0.5-2 μmol / m 2 .
[0019] Preferably, when preparing the modified organic silicon surfactant, 0.1-0.5% by mass of nano-silica aerogel is additionally added to the polydimethylsiloxane, polyether, and fluorocarbon chain reaction system.
[0020] Preferably, an antioxidant, di-tert-butylhydroquinone DTBHQ, is added to the mixed system in an amount of 0.01-0.05%, and nitrogen with a volume fraction of 0.5-2% is added as a protective gas.
[0021] Preferably, a high-efficiency stirring process of a silane mixed gas composite nanocatalysis-temperature-sensitive intelligent control system comprises the following steps:
[0022] S1: Raw material preparation, accurately weigh or measure silane, diluent gas, and various additives;
[0023] S2: Preparation of composite nanomaterials: disperse nano-tungsten carbide and graphene quantum dots in ethanol, add silane coupling agent KH550, stir at 50-70°C for 2-4 hours, and dry to obtain composite nanomaterials;
[0024] S3: Synthesis of modified surfactant: polydimethylsiloxane, allyl polyether, and fluorinated acrylate react at 80-120°C for 4-8 hours in the presence of a platinum catalyst, and nano-silica aerogel is added during the reaction;
[0025] S4: Preparation of thermosensitive microspheres: N-isopropylacrylamide as monomer and potassium persulfate as initiator, polymerized in water at 60-70°C for 3-5 hours to obtain thermosensitive polymer gel microspheres;
[0026] S5: microfluidic pretreatment, silane and part of the dilution gas are introduced into the microchannel reactor for preliminary mixing;
[0027] S6: Main mixing: introduce the pretreated gas into a container with a double-layer propeller stirrer at a stirring speed of 500-1500 rpm, introduce the remaining dilution gas, and simultaneously turn on the electric field-magnetic field synergy device;
[0028] S7: Adding additives: spraying composite nanomaterials, modified surfactant solution and temperature-sensitive microsphere suspension through a spray device with a spray pressure of 0.2-0.5 MPa and a particle size of 10-50 μm;
[0029] S8: aging treatment, continue stirring for 10-30 minutes, and let it stand at 10-30°C for 2-6 hours;
[0030] S9: Post-treatment, the mixed gas passes through a purification system equipped with molecular sieves, activated carbon and a low-temperature condensation device, with the temperature controlled at -10-20°C and a flow rate of 0.1-0.5L / min.
[0031] Preferably, the alternating magnetic field frequency in the electric field-magnetic field cooperative device is 50-100 Hz and the intensity is 0.1-0.5 T; the voltage of the DC electric field is 10-50 V / cm.
[0032] Preferably, the inner diameter of the microchannel reactor channel is 50-200 μm, and the flow rate of silane and part of the dilution gas is 0.1-1 mL / min.
[0033] Preferably, the drying in step S2 is performed by freeze drying, with a pre-freezing temperature of -40-30°C, a vacuum degree of 10-50 Pa, and a drying time of 12-24 hours.
[0034] Preferably, in step S6, the rotation speed of the inner blade of the agitator is 20-50% faster than that of the outer blade.
[0035] Preferably, in step S9, a gas concentration online monitoring device is connected in series after the purification system to detect the silane concentration in real time, and automatically feedback and adjust the mixing parameters when the deviation exceeds ±3%.
[0036] (3) Beneficial technical effects
[0037] Compared with the existing technology, the beneficial effects of the present invention are:
[0038] 1. By introducing a composite nanocatalyst of tungsten carbide nanoparticles and graphene quantum dots, the decomposition and uniform distribution of silane can be efficiently promoted at low temperatures. A specially modified organosilicon surfactant significantly reduces gas-gas interfacial tension and enhances gas dispersion. Thermosensitive polymer gel microspheres intelligently regulate gas molecular diffusion based on temperature changes. The synergistic effect of these three factors significantly improves the mixing uniformity of the silane gas mixture and significantly shortens mixing time. Compared to traditional processes, mixing uniformity is improved by over 50% and mixing time is reduced by 40%.
[0039] 2. The addition of antioxidants and protective gases effectively inhibits the oxidative decomposition of silane; antistatic agents eliminate static electricity risks during the mixing process; microfluidic pretreatment and electric-magnetic field coordinated control technology further reduce the risk of excessive local silane concentration, making the mixed gas more stable during storage and transportation, and reducing the explosion risk by more than 60%.
[0040] 3. Newly added electric-magnetic field coordinated regulation and microfluidic pretreatment technologies enable precise control of the mixing process. By adjusting the electric and magnetic field parameters, as well as the flow rate of the microfluidic reactor and other conditions, the mixing effect and performance of the mixed gas can be flexibly adjusted to meet the needs of different application scenarios. Furthermore, the online gas concentration monitoring device provides real-time feedback on the mixing status and automatically adjusts the mixing parameters to ensure stable mixed gas quality.
[0041] 4. The low-temperature catalytic system and efficient stirring design reduce energy consumption; the rational use of additives reduces silane waste and impurity generation, lowering subsequent purification costs. This process provides a high-quality, low-cost solution for preparing silane gas mixtures for industries such as semiconductors and photovoltaics, with broad application prospects and significant economic and social benefits. BRIEF DESCRIPTION OF THE DRAWINGS
[0042] Figure 1 This is a high-efficiency stirring process flow chart of a silane mixed gas composite nano-catalysis-temperature-sensitive intelligent control system proposed by the present invention;
[0043] Figure 2 is a line comparison chart of the mixing uniformity of the embodiment and the comparative example and the silane decomposition rate after storage for one month;
[0044] Figure 3 1 is a comparison chart of mixing time and unit mixed gas energy consumption of the embodiment and the comparative example;
[0045] Figure 4 It is a radar comparison chart produced after unifying the dimensions of the experimental results of the embodiment and the comparative example. DETAILED DESCRIPTION
[0046] according to Figures 1 to 4 , the specific implementation of the present invention is as follows:
[0047] Example 1
[0048] Raw material preparation: Measure 5% volume fraction of silane gas, and use hydrogen as a diluent gas to make up the remaining volume; weigh 0.05% of the total mass of the mixed system of nano-tungsten carbide and graphene quantum dot composite nanocatalyst (nano-tungsten carbide accounts for 40% by mass); prepare a modified silicone surfactant with a polyether group grafting rate of 15% and a fluorocarbon chain grafting rate of 5%, and add it in an amount of 0.1% of the total mass of the mixed system; weigh 0.2% of the total mass of temperature-sensitive polymer gel microspheres with a phase transition temperature of 25°C; add 0.01% of the total mass of the antioxidant di-tert-butylhydroquinone (DTBHQ), and prepare 0.5% by volume of nitrogen as a protective gas.
[0049] Preparation of composite nanocatalysts: Nano-tungsten carbide (particle size 5 nm) and graphene quantum dots (particle size 2 nm) were dispersed in 500 mL of anhydrous ethanol at a mass ratio of 4:6. 5 g of silane coupling agent KH550 was added and stirred at 50°C for 2 hours. After the reaction, the mixture was transferred to a freeze dryer and dried at a pre-freezing temperature of -40°C and a vacuum of 10 Pa for 12 hours. The mixture was then ground into a powder for later use.
[0050] Synthesis of modified silicone surfactant: 100 g of polydimethylsiloxane, 15 g of allyl polyether, 5 g of fluorinated acrylate, 5 ppm of platinum catalyst and 0.1 g of nano-silica aerogel were added to a reactor, and the temperature was raised to 80° C. and reacted for 4 hours to obtain a modified surfactant.
[0051] Preparation of thermosensitive microspheres: 10 g N-isopropylacrylamide and 0.05 g potassium persulfate were added to a three-necked flask, dissolved in 100 mL deionized water, and polymerized at 60°C for 3 hours under stirring. After the reaction, centrifugation, washing, and drying were performed to obtain thermosensitive polymer gel microspheres.
[0052] Microfluidic pretreatment: Silane and 20% hydrogen were introduced into a microchannel reactor with an inner diameter of 50 μm at a flow rate of 0.1 mL / min to form a microbubble dispersion system, which was then introduced into the main mixing container.
[0053] Main Mix: Evacuate the main mix container to a pressure below Pa, fill with argon to atmospheric pressure, and repeat three times. Turn on the double-layer propeller stirrer (the inner blade diameter is 1 / 3 of the container diameter, and the outer blade diameter is 2 / 3 of the container diameter) at a stirring speed of 500 rpm. Add the remaining hydrogen. Simultaneously, start an alternating magnetic field with a frequency of 50 Hz and an intensity of 0.1 T and a direct current electric field with a voltage of 10 V / cm.
[0054] Additive addition: The composite nanocatalyst and modified surfactant were prepared into a 5% ethanol solution, and sprayed into the container with the temperature-sensitive microsphere suspension through a spray device with a spray pressure of 0.2 MPa and a spray particle size of 10 μm.
[0055] Aging treatment: Continue stirring for 10 minutes and let it stand at 10°C for 2 hours.
[0056] Post-processing: The mixed gas is passed into a purification system equipped with molecular sieves, activated carbon and a low-temperature condensation device (temperature -10°C), with a flow rate controlled at 0.1L / min, and a gas concentration online monitoring device is connected in series for real-time detection.
[0057] Example 2
[0058] Raw material preparation: silane volume fraction is 15%, helium is the diluent gas; the addition amount of composite nanocatalyst is 0.3% (nano-tungsten carbide accounts for 50% by mass); modified silicone surfactant polyether group grafting rate is 20%, fluorocarbon chain grafting rate is 10%, and the dosage is 0.6%; the addition amount of thermosensitive microspheres is 0.8%, and the phase transition temperature is 30°C; the antioxidant DTBHQ accounts for 0.03% of the total mass, and the nitrogen protective gas volume fraction is 1.2%.
[0059] Preparation of composite nanocatalyst: Nano-tungsten carbide (particle size 12 nm) and graphene quantum dots (particle size 6 nm) were dispersed in 800 mL of anhydrous ethanol at a mass ratio of 1:1, and 8 g of silane coupling agent KH550 was added. The mixture was stirred at 60 °C for 3 h, pre-frozen at -35 °C, and freeze-dried under a vacuum of 20 Pa for 18 h.
[0060] Synthesis of modified organosilicon surfactant: 150 g polydimethylsiloxane, 30 g allyl polyether, 15 g fluorinated acrylate, 10 ppm platinum catalyst and 0.3 g nano-silica aerogel were added and reacted at 100 °C for 6 hours.
[0061] Preparation of thermosensitive microspheres: 15 g N-isopropylacrylamide, 0.1 g potassium persulfate, 120 mL deionized water, polymerization at 65 °C for 4 h.
[0062] Microfluidic pretreatment: the inner diameter of the microchannel was 120 μm, and the flow rate of the silane and helium mixture was 0.5 mL / min.
[0063] Main mixing: The diameter of the inner blade of the stirrer is 2 / 5 of the container diameter, the diameter of the outer blade is 3 / 5 of the container diameter, the stirring speed is 1000 rpm; the magnetic field frequency is 75 Hz, the intensity is 0.3 T, and the electric field voltage is 30 V / cm.
[0064] Additive addition: spray pressure 0.3 MPa, spray particle size 30 μm.
[0065] Aging treatment: Stir for 20 minutes and let stand at 20℃ for 4 hours.
[0066] Post-treatment: purification system temperature 0°C, flow rate 0.3 L / min.
[0067] Example 3
[0068] Raw material preparation: silane volume fraction 25%, hydrogen and helium 1:1 mixture as diluent gas; composite nanocatalyst addition amount 0.5% (nano-tungsten carbide mass proportion 60%); modified silicone surfactant polyether group grafting rate 30%, fluorocarbon chain grafting rate 15%, dosage 1%; temperature-sensitive microspheres addition amount 1.5%, phase transition temperature 35 ° C; antioxidant DTBHQ accounts for 0.05% of the total mass, nitrogen protective gas volume fraction 2%.
[0069] Preparation of composite nanocatalyst: Nano-tungsten carbide (particle size 20 nm) and graphene quantum dots (particle size 10 nm) were dispersed in 1000 mL of anhydrous ethanol and 10 g of silane coupling agent KH550 at a mass ratio of 6:4. The mixture was stirred at 70 °C for 4 h, pre-frozen at -30 °C, and freeze-dried at 50 Pa vacuum for 24 h.
[0070] Synthesis of modified organosilicon surfactant: 200 g polydimethylsiloxane, 60 g allyl polyether, 30 g fluorinated acrylate, 20 ppm platinum catalyst and 1 g nano-silica aerogel were reacted at 120 °C for 8 h.
[0071] Preparation of thermosensitive microspheres: 20 g N-isopropylacrylamide, 0.3 g potassium persulfate, 150 mL deionized water, polymerization at 70 °C for 5 h.
[0072] Microfluidic pretreatment: microchannel inner diameter 200 μm, mixture flow rate 1 mL / min.
[0073] Main mixing: the diameter of the inner blade is 1 / 2 of the container diameter, the diameter of the outer blade is 3 / 4 of the container diameter, the stirring speed is 1500 rpm; the magnetic field frequency is 100 Hz, the intensity is 0.5 T, and the electric field voltage is 50 V / cm.
[0074] Additive addition: spray pressure 0.5 MPa, spray particle size 50 μm.
[0075] Aging treatment: Stir for 30 minutes and let stand at 30℃ for 6 hours.
[0076] Post-treatment: purification system temperature 20°C, flow rate 0.5 L / min.
[0077] Comparative Example
[0078] Raw material preparation: 15% volume fraction of silane gas was measured, and helium was used as the diluent gas; ordinary polydimethylsiloxane surfactant was weighed and added in an amount of 0.6% of the total mass of the mixed system; no composite nanocatalyst, temperature-sensitive polymer gel microspheres, and antioxidant were added.
[0079] Mixing process: After briefly cleaning the mixing container, directly introduce silane and helium, use a common paddle stirrer, stir at a speed of 300 rpm, and stir at room temperature for 30 minutes.
[0080] Post-processing: After mixing, the mixture was filtered through a common filter without deep purification and monitoring. The experimental results of the embodiment and the comparative example are compared in the following table:
[0081] Table 1
[0082]
[0083] Conclusion: The above examples and comparative examples demonstrate that the examples, using the technology of the present invention, significantly outperform the comparative examples in terms of mixing uniformity, stability, and safety. Although Example 3 has higher energy consumption, it achieves the best mixing effect, demonstrating that the process of the present invention can effectively improve the quality of silane mixed gas and meet the needs of high-end applications.
[0084] While embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions, and variations may be made to these embodiments without departing from the principles and spirit of the invention, and that the scope of the invention is defined by the appended claims and their equivalents.
Claims
1. A silane mixed gas composite nanocatalysis-temperature sensitive intelligent control system, characterized in that: The invention comprises silane, a diluent gas, a nanocatalyst composed of nano-tungsten carbide and graphene quantum dots (GQDs), a modified organic silicon surfactant, and temperature-sensitive polymer gel microspheres as intelligent control additives; the diluent gas is hydrogen, helium, or a mixture of the two; the mass of nano-tungsten carbide in the composite nanomaterial accounts for 40-60%, and the addition amount is 0.05-0.5% of the total mass of the mixed system; the volume fraction of silane in the mixed gas is 5-25%; the modified organic silicon surfactant is made of polydimethylsiloxane grafted with polyether groups and fluorocarbon chains, the addition amount is 0.1-1%, the polyether group grafting rate is 15-30%, and the fluorocarbon chain grafting rate is 5-15%; the temperature-sensitive polymer gel microspheres use N-isopropylacrylamide as a monomer; the structural formula of the polydimethylsiloxane is: The structural formula of polyether group grafted polydimethylsiloxane is: The structural formula of fluorocarbon chain grafted polydimethylsiloxane is: 。 2. The silane mixed gas composite nanocatalysis-temperature sensitive intelligent control system according to claim 1, characterized in that: The nano-tungsten carbide particle size is 5-20 nanometers, and the graphene quantum dot particle size is 2-10 nanometers. The surfaces of both are amino-treated, and the amino density is 0.5-2 μmol / m 2 .
3. The silane mixed gas composite nanocatalysis-temperature sensitive intelligent control system according to claim 1, characterized in that: When preparing the modified organic silicon surfactant, 0.1-0.5% by mass of nano-silica aerogel is additionally added to the polydimethylsiloxane, polyether and fluorocarbon chain reaction system.
4. The silane mixed gas composite nanocatalysis-temperature sensitive intelligent control system according to claim 1, characterized in that: The antioxidant di-tert-butylhydroquinone DTBHQ is added to the mixed system in an amount of 0.01-0.05%, and nitrogen with a volume fraction of 0.5-2% is filled in as a protective gas.
5. The efficient stirring process of the silane mixed gas composite nanocatalysis-temperature sensitive intelligent control system according to claim 4, characterized in that: The following steps are involved: S1: Raw material preparation, accurately weigh or measure silane, diluent gas, and various additives; S2: Preparation of composite nanomaterials: disperse nano-tungsten carbide and graphene quantum dots in ethanol, add silane coupling agent KH550, stir at 50-70°C for 2-4 hours, and dry to obtain composite nanomaterials; S3: Synthesis of modified surfactant: polydimethylsiloxane, allyl polyether, and fluorinated acrylate react at 80-120°C for 4-8 hours in the presence of a platinum catalyst, and nano-silica aerogel is added during the reaction; S4: Preparation of thermosensitive microspheres: N-isopropylacrylamide as monomer and potassium persulfate as initiator, polymerized in water at 60-70°C for 3-5 hours to obtain thermosensitive polymer gel microspheres; S5: microfluidic pretreatment, silane and part of the dilution gas are introduced into the microchannel reactor for preliminary mixing; S6: Main mixing: introduce the pretreated gas into a container with a double-layer propeller stirrer at a stirring speed of 500-1500 rpm, introduce the remaining dilution gas, and simultaneously turn on the electric field-magnetic field synergy device; S7: Adding additives: spraying composite nanomaterials, modified surfactant solution and temperature-sensitive microsphere suspension through a spray device with a spray pressure of 0.2-0.5 MPa and a particle size of 10-50 μm; S8: aging treatment, continue stirring for 10-30 minutes, and let it stand at 10-30°C for 2-6 hours; S9: Post-treatment, the mixed gas passes through a purification system equipped with molecular sieves, activated carbon and a low-temperature condensation device, with the temperature controlled at -10-20°C and a flow rate of 0.1-0.5L / min.
6. The efficient stirring process of the silane mixed gas composite nanocatalysis-temperature sensitive intelligent control system according to claim 5, characterized in that: The alternating magnetic field frequency in the electric field-magnetic field cooperative device is 50-100 Hz and the intensity is 0.1-0.5 T; the voltage of the direct current electric field is 10-50 V / cm.
7. The efficient stirring process of the silane mixed gas composite nanocatalysis-temperature sensitive intelligent control system according to claim 5, characterized in that: The inner diameter of the microchannel reactor channel is 50-200 μm, and the flow rate of silane and part of the dilution gas is 0.1-1 mL / min.
8. The efficient stirring process of the silane mixed gas composite nanocatalysis-temperature sensitive intelligent control system according to claim 5, characterized in that: In step S2, the drying is carried out by freeze drying, with a pre-freezing temperature of -40-30°C, a vacuum degree of 10-50 Pa, and a drying time of 12-24 hours.
9. The efficient stirring process of the silane mixed gas composite nanocatalysis-temperature sensitive intelligent control system according to claim 5, characterized in that: In step S6, the speed of the inner blade of the stirrer is 20-50% faster than that of the outer blade.
10. The efficient stirring process of the silane mixed gas composite nanocatalysis-temperature sensitive intelligent control system according to claim 5, characterized in that: In step S9, a gas concentration online monitoring device is connected in series after the purification system to detect the silane concentration in real time. When the deviation exceeds ±3%, the mixing parameters are automatically adjusted through feedback.
Citation Information
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