44results about "Silicon hydrides" patented technology

The system comprises a gradient catalytic reaction rectifying tower and a temperature control system, the rectifying tower is sequentially provided with a rectifying section, a reaction section and a stripping section from top to bottom, the reaction section is filled with an ion exchange resin solid catalyst, and the stripping section is filled with an ion exchange resin solid catalyst. The radiuses of the catalyst bag units are distributed in a gradient mode from small to large along the height of the tower, the catalyst bag units have the functions of catalytic reaction and mass transfer separation, the rectifying section and the stripping section are filled with structured packing or high-separation-capacity metal wire mesh packing, a gas-liquid separator is arranged at an outlet of the stripping section, and a temperature control system achieves segmented monitoring through a multi-point temperature sensor. The surface of the catalyst can be subjected to functional treatment to improve the decomposition resistance; the method comprises the following steps: feeding trichlorosilane generated by cold hydrogenation into the upper part of a reaction section from a feed port, carrying out disproportionation reaction at the gradient temperature of 20-100 DEG C and the pressure of 0.3-0.6 MPa according to the reflux ratio of (15-30): 1 to generate silane, and carrying out rectification and extraction separation to obtain high-purity silane with the purity of 99.999% or above.

The application discloses a process and equipment for producing silane by chlorosilane disproportionation with combined solid catalyst and liquid catalyst, and the process at least comprises a reaction rectification stage catalyzed by a solid catalyst and a reaction and separation stage catalyzed by a liquid catalyst. The process of the application uses the solid catalyst and the liquid catalyst simultaneously, and combines the homogeneous catalytic reaction rectification and the heterogeneous catalytic reaction rectification, so that the rate-controlling step of the disproportionation reaction is first balanced through primary disproportionation, then the generated intermediate product is subjected to secondary disproportionation, and the silane and the silicon tetrachloride are continuously removed, so that the chemical equilibrium is further transferred to the product site, that is, the limited reaction conversion of the very high or all chemical equilibrium is achieved. The chlorosilane disproportionation reaction which is not favorable to the reaction kinetics is strengthened, the reaction is promoted to reach the equilibrium, and the multiple disproportionation is used to improve the reaction conversion rate.

The utility model provides an impurity removal system for preparing disproportionation reaction silane gas, which comprises a dehydrogenation tower (1) for preparing silane, and further comprises a side production pipeline (5) arranged in the middle of the side of the dehydrogenation tower (1), the other end of the side production pipeline (5) is in fluid connection with a circulating water condenser (6), and the other end of the circulating water condenser (6) is in fluid connection with the dehydrogenation tower (1). A liquid phase outlet of the circulating water condenser (6) is in fluid connection with a buffer tank (7), and the buffer tank (7) is in fluid connection with a silane reaction tower (9) through a pump (8). According to the device, the content of heavy phosphorus impurities in silane gas can be reduced, and the quality of the product silane gas is improved; the dehydrogenation tower is transformed to reduce the influence of phosphorus impurities on the activity of the catalyst in the reaction tower.

The utility model relates to the technical field of chemical equipment, and discloses a disilane preparation device, which comprises a mounting plate, the supporting block is arranged on the mounting plate; the clamping sleeve is fixedly arranged above the supporting block; the reaction kettle is fixedly arranged in the jacket; the feeding hole is formed in the reaction kettle, and a feeding pipe is fixedly arranged in the feeding hole; the outlet is formed in the reaction kettle and is formed in one side of the feeding hole, and a discharging pipe is fixedly connected to the outlet; the gas inlet hole is formed in the reaction kettle, and the output end of a gas compressor is fixedly connected to the interior of the gas inlet hole; the stirring mechanism is arranged in the reaction kettle; the slag discharge pipe is communicated with the jacket and the reaction kettle, and the slag discharge pipe is arranged at the bottom of the reaction kettle; the rectifying tower is communicated with the discharging pipe, the top of the rectifying tower is connected with a condenser, the bottom of the rectifying tower is connected with a reboiler, and the rectifying tower is communicated with a storage tank. The disilane preparation device disclosed by the utility model is used for solving the problems of the existing equipment.

The invention discloses a high-purity disilane production system and a high-purity disilane production method. The system comprises a reactor (100), a primary gas-solid separator (200), supercharging equipment (300), a secondary gas-solid separator (400), a gas separation membrane assembly (500), a light component removal tower (600) and a product tower (700) which are sequentially connected through pipelines. The core of the invention lies in that a two-stage gas-solid separation structure is adopted to effectively solve the contradiction between the low-pressure operation of the reactor and the high-pressure feeding of the membrane module, and core equipment is fully protected; meanwhile, a mixed matrix molecular sieve membrane is arranged in the gas separation membrane assembly, and screening of hydrogen and monosilane molecules can be efficiently achieved, so that the reaction byproduct hydrogen is removed through a one-step method. According to the method, monosilane is taken as a raw material, after reaction synthesis, primary dust removal, pressurization, fine dust removal, membrane-method dehydrogenation and rectification separation are sequentially carried out on a product, a high-purity disilane product is finally obtained, and unreacted monosilane is returned to a system for cyclic utilization.

Disclosed are Group V element-containing precursors, methods for their synthesis, and methods for their use in film deposition. The precursor is (SiR3) 3-m A(Si a H 2a+1 ) m , (SiR3) 3-n-p A(Si a H 2a+1 ) n (Si b H 2b+1 ) p , or A(Si a H 2a+1 )(Si b H 2b+1 )(Si c H 2c+1 ) (wherein a=1-6; b=1-6; c=1-6; a≠b≠c; m=1-3; n=1-2, p=1-2, n+p=2-3; A=As, P, Sb, Bi; R is C1-C 10 (A is selected from linear, branched, or cyclic alkyl, alkenyl, alkynyl groups of A). Synthesis methods include one-step, two-step, or three-step reaction between halo(poly)silanes and tris(trialkylsilyl) derivatives of A, or one-pot mixture reaction of two or three halo(poly)silanes with a mixture of tris(trialkylsilyl) derivatives of A. Deposition methods include CVD, PECVD, ALD, PEALD, flowable CVD, HW-CVD, epitaxy, etc.

The utility model provides a monosilane buffer filling device which comprises a condenser (7) used for converting gaseous monosilane into liquid monosilane, the input end of the condenser (7) is the input end of the device, and the outlet of the condenser (7) is in fluid connection with a hollow monosilane buffer tank (3) used for storing monosilane. The monosilane buffer tank (3) is in fluid connection with the vaporizer (4) and used for converting liquid monosilane in the monosilane buffer tank (3) into a gas state, and the monosilane buffer tank (3) is provided with a gas state outlet, namely the output end of the device.

The invention relates to a method and a device for gas-phase continuous preparation of disilane. The method comprises the following steps: S1, gas phase catalytic reaction-hydrogen separation integration: introducing a silane raw material into a tubular reactor filled with a palladium separation membrane, and carrying out a gas phase dehydrogenation condensation reaction under the action of the palladium separation membrane to obtain a component I and a component II; and S2, separation of silane, disilane and trisilane: carrying out three-stage separation on the component II to obtain disilane. The device comprises a catalytic reaction-separation integrated fixed bed device, a first distillation tower, a second distillation tower and a third distillation tower which are arranged along the material flow direction. The palladium separation membrane has the characteristics of catalytic activity and hydrogen separation function, the single-pass yield and selectivity of disilane are improved, generation of trisilane and deposition of silicon powder are inhibited, meanwhile, efficient utilization of raw materials is achieved, the reaction time is short, and no liquid or gas waste is generated in the whole process.

The utility model discloses a production device for improving the purity of silane, which comprises a first heat exchanger which is sequentially connected with a primary purification component and a secondary purification component through a pipeline, the primary purification assembly comprises a first resin column used for carrying out liquid phase adsorption on liquid silane and a first rectifying tower used for carrying out rectification separation on the silane, and the secondary purification assembly comprises a second resin column used for carrying out gas phase adsorption on silane gas and a second rectifying tower used for carrying out rectification separation on the silane. According to the utility model, two purification operations of resin complexing adsorption and rectification are combined for the first time, and the permutation and combination of rectification and complexing adsorption are optimized again, so that the purpose of removing impurities is achieved. According to the process, the removal and rectification load of trace impurities by single rectification operation is greatly reduced, and the rectification pressure and energy consumption can be effectively reduced.

The invention discloses a preparation method of high-purity silane suitable for a small experimental device, which comprises the following steps: sequentially connecting and arranging a main reactor, a second reactor, a condenser, a silane buffer tank, a booster pump and a silane steel cylinder, and injecting hydrogen, nitrogen and silicon tetrafluoride materials into the main reactor after passing through the same mass flow controller; then the material enters a second reactor through a gas phase outlet pipeline at the top of the main reactor, a gas phase outlet at the top of the second reactor is connected with an inlet at the bottom of a condenser, an outlet of the condenser is connected with a silane buffer tank, and an outlet pipeline is arranged at the top of the silane buffer tank; materials enter the booster pump through the outlet pipeline, are pressurized in the booster pump and then are fed into the silane steel cylinder to be stored, so that the complexity of the reaction device is simplified, the energy consumption is reduced, and the problems of huge device size, complex process conditions and the like are solved.

The utility model relates to the technical field of silane production, in particular to an electronic-grade silane system device which comprises a partition plate tower, the partition plate tower is communicated with a purification furnace through a first pipeline, the purification furnace is connected with a rectifying tower through a second pipeline, and a filter is arranged on the second pipeline. Process gas prepared by a silicon-magnesium method reaction kettle is conveyed to the middle of a partition plate tower, light component impurities such as H2 and N2 are removed at the top of the partition plate tower, and after non-metal hydride and high-order silane components such as silane and disilane are removed at the bottom of the tower, crude silane is extracted from the tower side and is introduced into a purification furnace through a first pipeline, and by means of the property that the thermal stability of the silane and the hydride impurities is different, the high-order silane is obtained. And adjusting the temperature of the purification furnace to a proper temperature, carrying out thermal decomposition on hydride impurities, filtering a silane gas phase obtained in the purification furnace through a filter on a second pipeline, introducing the filtered silane gas phase into a rectifying tower for refining, and finally extracting a liquid phase, thereby obtaining the high-purity electronic-grade silane.

The utility model provides a preparation device of electronic-grade silane. According to the preparation device, a first disproportionation reaction is carried out on the basis of the first reactor, dichlorosilane is rectified and separated to serve as a raw material for a second disproportionation reaction, silane can be obtained on the basis of cheap trichlorosilane and a catalytic reagent, and electronic-grade silane can be obtained on the basis of traditional purification after rectification; based on heat exchange between tower top materials of the rectifying tower I and a tower kettle reboiler of the rectifying tower II, differential pressure thermal coupling integration is realized, condensing equipment and operation steps can be omitted, energy consumption is reduced, and the defects of high preparation cost and high energy consumption of a silane preparation device in the prior art are overcome.

This invention discloses a single-atom catalyst for the disproportionation of SiHCl3 to SiH4 and its preparation method. The catalyst uses a transition metal as the active center, with single atoms dispersed on a high-temperature resistant support. High metal loading (0.5~5 wt%) and stable dispersion are achieved through coordination anchoring or high-temperature pyrolysis. This catalyst possesses single-atom active sites and strong interactions between the metal and the support, improving reactivity and SiH4 selectivity. The preparation method employs scalable technology, ensuring uniform distribution and stability of single atoms by optimizing the precursor ratio and heat treatment conditions. This catalyst achieves high SiHCl3 conversion and high SiH4 selectivity at relatively low temperatures (150~300℃), and has a long lifespan, making it suitable for continuous industrial production. It offers advantages such as high efficiency, low energy consumption, and long-term operation.

The invention discloses a system for purifying impurity gas in a disilane product synthesized from silane. The system comprises a membrane separation device, a fan, a first rectifying tower and a second rectifying tower which are communicated in sequence, the invention further relates to a process for purifying the impurity gas in the product of synthesizing the disilane from the silane, high-content hydrogen and other light components in the product gas of synthesizing the disilane from the silane are primarily separated from the silane, the disilane and the trisilane by adopting a membrane separation mode, then rectification separation is carried out, the purity of the recovered disilane is up to 99.995% or above, the purity of the recovered disilane is up to 99.995% or above, the purity of the recovered disilane is up to 99.995% or above, and the purity of the recovered disilane is up to 99.995% or above. The process is efficient, simple and low in energy consumption.

The application provides a silane gas production system and method based on double reaction distillation columns. The system comprises a second reaction distillation column (2) arranged in the silane gas production system, a middle input end of the second reaction distillation column (2) is connected with a bottom output end of a silane distillation column (3) in the silane gas production system, receives an intermediate mixture output from the silane distillation column (3) and performs a disproportionation reaction; a top output end of the second reaction distillation column (2) is connected with a top output end of a first reaction distillation column (1) in the silane gas production system, and the mixture in the second reaction distillation column (2) is subjected to subsequent treatment; and a bottom output end of the second reaction distillation column (2) is connected with a middle input end of the first reaction distillation column (1) in the silane gas production system, and the output from the first reaction distillation column (1) is subjected to a disproportionation reaction. The method is realized by using the system to produce silane gas based on double reaction distillation columns.

The object of the present invention is to provide a method for producing a silicon film having high uniformity of film thickness or high step coverage through reduction of the thermal history of a cyclic silane compound. The present invention relates to a method for producing a silicon film, including the steps of heating a substrate inserted into a reactor of a cold-wall type thermal CVD system, supplying the cyclic silane compound to the reactor, and forming the silicon film on the substrate.

The invention discloses a production method for preparing monosilane gas by using chlorosilane, and belongs to the technical field of monosilane preparation, which comprises the following steps: preheating chlorosilane, and removing light component impurities; cooling the first tower kettle produced liquid subjected to impurity removal, and then carrying out secondary impurity removal; the material subjected to secondary impurity removal is subjected to a first reaction and a second reaction after passing through a second preheater, is subjected to first condensation after the first reaction and then flows back to the reaction tower, is subjected to second condensation after the second reaction and then flows back to the reaction tower, and the reacted material is discharged from the top of the reaction tower, is subjected to second cooling and then partially flows back; the other part enters a chlorosilane rectifying tower; a tower top produced liquid part of the reaction tower is subjected to rectification separation, a tower top produced liquid of the chlorosilane rectifying tower is subjected to secondary rectification, monosilane containing light component impurities is discharged through the tower top of the product rectifying tower, a monosilane product is produced through the side part of the product rectifying tower, and a tower kettle produced liquid of the product rectifying tower is discharged. According to the method, chlorosilane is utilized, and monosilane is prepared after simple treatment.

The invention discloses a process and system for producing electronic-grade silane through thermal coupling reactive distillation, and relates to the technical field of electronic-grade silane generation, and the system mainly comprises a reactive distillation tower, a compression system, a silane crude distillation tower, a silane refining tower, a silane adsorption tower, a solvent recovery tower, a tail gas treatment system and a filtering and drying system. According to the technology, silicon tetrafluoride gas and a sodium aluminum hydride solution are introduced into a reactive distillation tower for a reverse contact reaction, generated crude silane gas is subjected to compression, multi-stage distillation and adsorption purification, and finally 9N-12N electronic-grade silane is obtained. A stirring kettle is replaced by reactive distillation, so that the risk of dynamic seal leakage is thoroughly eliminated; by adopting a multi-stage thermal coupling technology, reaction heat, tower bottoms and compression heat are used for heating the system, so that the energy consumption is obviously reduced; the method realizes cyclic utilization of the solvent and fluorine resources, and has the advantages of high safety, high product purity, low energy consumption and comprehensive utilization of resources.

The application relates to a method for separating hydrogen / silane, in particular to a method for separating hydrogen / silane at high temperature by using a molecular sieve membrane. The application uses a molecular sieve membrane as a key membrane material, realizes the separation of hydrogen and silane at high temperature, and the high-temperature environment of a specific temperature can also modify the membrane defects of the molecular sieve membrane, so that the separation performance of the membrane for hydrogen and silane is improved.

The utility model belongs to the technical field of rectification equipment, and particularly relates to a disilane multi-stage rectification purification device which comprises a bottom plate, a rectification tower body, a tower bottom product cooler, a reboiler and a tower top product cooler are arranged at the top of the bottom plate, a packed tower is arranged at the top of the rectification tower body, and a mounting frame is arranged at the top of the packed tower. The top of the mounting rack is provided with a condenser, and the mounting rack is connected with the packed tower and the condenser through a mounting structure; a lower mounting assembly; wherein the upper mounting assembly and the lower mounting assembly have the same structure and are symmetrically arranged at the two ends of the mounting frame, the two ends of the upper mounting assembly are connected with the mounting frame and the packed tower, and the two ends of the lower mounting assembly are connected with the mounting frame and the condenser. The device has the beneficial effects that by arranging the mounting structure, a worker can more conveniently and rapidly assemble and disassemble the device, the problem of thread abrasion is reduced, and the assembling efficiency is improved.

The application provides a purification system and method of electronic-grade silane, and belongs to the technical field of high-purity special gas purification. The purification system comprises a raw material pretreatment unit, a directional adsorption unit, a coupled rectification unit and a membrane separation unit connected in sequence; the directional adsorption unit comprises an adsorption tower filled with a composite adsorbent; the coupled rectification unit comprises a low-temperature rectification section and a normal-temperature rectification section; the membrane separation unit comprises a primary membrane assembly and a secondary membrane assembly arranged in series; the composite adsorbent is composed of citric acid modified NaA type zeolite and MOF-303; the volume ratio of the citric acid modified NaA type zeolite and the MOF-303 is 2.5:1-3.5:1. The application adopts an innovative three-stage purification process of directional adsorption-coupled rectification-membrane separation, realizes efficient purification of electronic-grade silane, the purity of the product is greater than or equal to 99.9999%, and the contents of key electrically active impurities boron and phosphorus are both less than or equal to 0.1 ppb.

The invention provides an electronic-grade silane purification system and method, and belongs to the technical field of high-purity special gas purification. The purification system comprises a raw material pretreatment unit, a directional adsorption unit, a coupling rectification unit and a membrane separation unit which are connected in sequence, the directional adsorption unit comprises an adsorption tower filled with a composite adsorbent; the coupling rectification unit comprises a low-temperature rectification section and a normal-temperature rectification section; the membrane separation unit comprises a first-stage membrane assembly and a second-stage membrane assembly which are arranged in series; the composite adsorbent is prepared from citric acid modified NaA type zeolite and MOF-303; the volume ratio of the citric acid modified NaA type zeolite to the MOF-303 is (2.5: 1)-(3.5: 1). According to the method, an innovative three-stage purification process of directional adsorption, coupled rectification and membrane separation is adopted, efficient purification of electronic-grade silane is achieved, the product purity is larger than or equal to 99.9999%, and the content of key electroactive impurities boron and phosphorus is smaller than or equal to 0.1 ppb.

The invention relates to the technical field of silane purification, and provides a method for removing impurity ammonia in silane, and by adopting the method, the risk of equipment blockage can be reduced, and the operation cycle of equipment can be remarkably prolonged. The method comprises the following steps: (1) feeding crude silane gas containing impurity ammonia into a rectifying tower for rectification, wherein the pressure of the rectifying tower is 0.12-2Mpa, the tower top temperature is less than or equal to-10 DEG C, and the tower kettle temperature is more than or equal to 10 DEG C; (2) feeding the silane gas subjected to rectification treatment in the step (1) into a rectification condensation tank, and condensing under the conditions that the temperature is-40 DEG C to-90 DEG C and the pressure is 0.13-1.9 Mpa; (3) feeding the silane gas treated in the step (2) into a solidification separator, and condensing under the conditions that the temperature is-80 DEG C to-160 DEG C and the pressure is 0.14-1.85 Mpa; nitrogen is introduced into a liquid phase obtained through condensation in the solidification separator in the condensation process; and filtering the liquid phase in the solidification separator to obtain purified silane.

According to the preparation device of the electronic-grade disilane, high-order silane is generated on the basis of pyrolysis polymerization reaction of crude monosilane, after the high-order silane is primarily separated by the circulating tower, heavy components are rectified twice to remove light components and heavy components respectively, and then are purified twice to remove water, oxygen and metal ions to obtain the electronic-grade disilane, so that continuous production is realized, the production cost is reduced, and the production efficiency is improved. And common unit equipment combination can be directly used, so that the cost is low, the efficiency is high, and a new choice is provided for preparation of electronic-grade disilane.

The invention relates to the technical field of gas separation and purification, in particular to a method for recycling hydrogen in silane and disilane mixed gas through a membrane separation method. Comprising the following steps: S1, pretreating mixed gas containing 20%-25% of silane, 10%-15% of disilane and 60%-70% of hydrogen to remove solid particles and moisture; s2, the pretreated mixed gas is introduced into a membrane separation device, silane and disilane are collected on the enrichment side of the membrane separation device for further rectification, and hydrogen is collected on the permeation side of the membrane separation device for further purification. According to the method, hydrogen recovery and silane and disilane enrichment can be efficiently achieved, the hydrogen recovery rate is high, and compared with a traditional separation method, the method is low in energy consumption and has remarkable economic benefits and environmental protection benefits.

The invention discloses a system and a method for recovering and purifying silane in particle silicon production tail gas, relates to the technical field of silane recovery processes, and aims to solve the problems of silane waste and the like due to neglect of ethane and ethylene accumulation and desorption in the particle silicon production tail gas recovery process in the prior art. The device comprises a heat exchange condensation unit, a decarburization unit and an adsorption and desorption unit, the heat exchange condensation unit is used for converting the particle silicon production tail gas into silane liquid through heat exchange condensation; the decarburization unit is used for removing and recovering methane from the silane liquid, the adsorption and desorption unit is used for removing ethane and ethylene in the silane liquid subjected to methane removal to obtain purified silane, and the ethane and the ethylene are desorbed after adsorption saturation. According to the method, the silane is purified by adsorbing the ethane and the ethylene in the silane recovery process, the problem of accumulation of trace impurities of the ethane and the ethylene is solved, the desorption process after the ethane and the ethylene are adsorbed is optimized, the loss of the silane is further reduced, the treatment cost of exhaust gas is reduced, and the production benefit of granular silicon is effectively improved.

The present invention relates to a silane recovery device and method and, more specifically, is to provide a silane recovery device and method, which enable the recovery and recycling of silane by efficiently removing impurities such as hydrogen, nitrogen, etc., from silane gas, which is an unreacted by-product generated from processes using silane as a raw material in the fields of silane manufacturing facilities or semiconductors, displays, batteries, etc.

The invention discloses a comprehensive production method of high-purity crystalline silicon. Specifically, the smelting process of industrial silicon is incorporated into a production system, so that the product can be better traced, the product quality is controlled from the source, the doping of impurities is reduced, and a good foundation is laid for the subsequent production of high-purity crystalline silicon. The flue gas generated in the industrial silicon smelting process is converted into high-pressure steam, energy is provided for follow-up production, compared with independent production, the energy utilization rate is increased, energy waste is reduced, the requirements of low energy consumption and environmental protection are better met, and compared with an improved Siemens method and a fluidized bed method, the comprehensive power consumption of high-purity crystalline silicon is smaller than 15 kWh / kg. The byproduct dichlorosilane is separated to extract the generated monosilane, and the monosilane can be decomposed to obtain granular silicon, so that the conversion efficiency of the silicon element is further increased, and the comprehensive silicon conversion rate is greater than 99%. The deposition efficiency of the silicon element is greatly improved, and the purity of the polycrystalline silicon reaches an electronic grade of 99.999999999%.

The invention discloses a large ten-thousand-ton superfine silicon nitride powder production method which is characterized by comprising the following steps: S1, carrying out disproportionation reaction on trichlorosilane to generate a mixture containing silane and silicon tetrachloride, and separating and purifying the mixture to respectively obtain high-purity silane and high-purity silicon tetrachloride; s2, enabling the silane obtained in the step S1 to react with ammonia gas in a fluidized bed reactor to obtain a target product silicon nitride, a byproduct hydrogen and excessive ammonia gas, and collecting the silicon nitride, the hydrogen and the ammonia gas; s3, the silicon tetrachloride obtained in the step S1, the hydrogen obtained in the step S2 and silicon powder are subjected to a cold hydrogenation reaction, and trichlorosilane is regenerated; and S4, returning the trichlorosilane generated in the step S3 to the step S1 for recycling. The system is a closed reaction system, silane is prepared, the production cost is reduced, and mass production is facilitated.

The invention relates to a method for coating cylinder liners in the cylinder bores (2) of crankcases (1) for internal combustion engines, wherein the coating is applied by means of arc wire spraying, wherein an inert atomizing gas and a silane-containing additive are used for the arc wire spraying.