69 results about "Nitrogen trifluoride" patented technology

The invention belongs to the field of chemical purification, and discloses a method and equipment for separating carbon tetrafluoride in nitrogen trifluoride through pressurized absorption of a deep eutectic solvent, and the method comprises the following steps: (1) increasing the pressure of nitrogen trifluoride crude gas to 0.5 MPa or above; (2) cooling the crude gas to below 40 DEG C through a crude gas feeding heat exchanger; (3) through the absorption tower, the crude gas entering from the tower kettle is in countercurrent contact with the eutectic solvent entering from the tower top, and the content of carbon tetrafluoride in the crude gas is reduced to 5 ppm or below; (4) reducing the content of carbon tetrafluoride in the eutectic solvent to be less than 1ppm through a two-stage flash tank; and (5) reducing the temperature of the eutectic solvent to be below 30 DEG C through a eutectic solvent discharging heat exchanger and a eutectic solvent cooler, and circulating the eutectic solvent back to the absorption tower from the bottom of the absorption tower. According to the method, the quality of the nitrogen trifluoride product can be improved, the carbon tetrafluoride impurity in the nitrogen trifluoride purity can be reduced to 5ppm, and the cost is low.

The invention relates to a preparation method of octafluorocyclobutane, which comprises the following steps: mixing hexafluorocyclobutene with preheated nitrogen trifluoride, carrying out addition reaction on the mixed gas, and condensing and collecting the octafluorocyclobutane after the reaction is completed. According to the method, octafluorocyclobutane is prepared by using nitrogen trifluoride, continuous production of octafluorocyclobutane with the purity being 99 wt% or above can be achieved, the preparation method has the advantages of being low in raw material cost, simple in process, low in energy consumption, simple in product separation, good in selectivity and convenient to purify, and amplified continuous production can be achieved easily.

The invention relates to a preparation method of antimony pentafluoride, which comprises the following steps: preheating raw material gas nitrogen trifluoride, placing nitrogen trifluoride and antimony powder in a tubular furnace reactor made of a specific material, carrying out gradient heating reaction at 300-400 DEG C under the condition that the antimony powder is distributed by adopting a multi-layer nickel plate tiled structure, carrying out reaction for 10-40 seconds, and carrying out solid filtration through a filter after the reaction is completed, so as to obtain the antimony pentafluoride. And carrying out cold trap collection to obtain an antimony pentafluoride product. The diameter of the reactor is made of a nickel material or Monel to prevent corrosion of antimony pentafluoride, the number of tiled layers of nickel plates is r / 5-r / 10, the contact area is increased, the reaction yield is increased, and the utilization rate of the raw material nitrogen trifluoride is increased.

The invention provides a process for purifying nickel from electrolytic waste for preparing nitrogen trifluoride, which comprises the following steps: after a nitrogen trifluoride electrolytic cell stops electrolysis, transferring the electrolytic waste into a first batching kettle, adding anhydrous hydrogen fluoride, dissolving ammonium bifluoride mixed in the electrolytic waste into a molten state, and adding a second batching kettle; then solid-liquid separation is achieved in a centrifugal mode, and the liquid part is molten liquid to be reused as electrolyte; ammonia water is added into a second batching kettle to adjust the pH value, solid-liquid separation is achieved in a centrifugal mode, the liquid part is transferred into an intermediate tank, potassium hydroxide is added to continue to adjust the pH value, nickel in the solution is precipitated out, ammonia escapes and is prepared into dilute ammonia water in a falling film absorption mode, and the dilute ammonia water can return to a system to be reused; the solid part directly enters a smelting furnace, the temperature is gradually increased until nickel is smelted into a liquid state, then cooling is conducted, and the nickel purity can reach 99% or above. According to the method, the nickel in the electrolytic waste mixed with the sediments in the nitrogen trifluoride electrolytic cell is purified, and appreciation is achieved.

The application belongs to the field of chemical purification, and discloses a method for separating carbon tetrafluoride in nitrogen trifluoride by using a eutectic solvent under pressure and an equipment thereof, which comprises the following steps: (1) increasing the pressure of crude nitrogen trifluoride gas to more than 0.5 MPa; (2) cooling the temperature of the crude gas to below 40 DEG C through a crude gas feeding heat exchanger; (3) reducing the content of carbon tetrafluoride in the crude gas to below 5 ppm by countercurrent contact between the crude gas entering the tower kettle and the eutectic solvent entering the top of the absorption tower through the absorption tower; (4) reducing the content of carbon tetrafluoride in the eutectic solvent to below 1 ppm through two-stage flash tanks; and (5) reducing the temperature of the eutectic solvent to below 30 DEG C through a eutectic solvent discharging heat exchanger and a eutectic solvent cooler, and circulating the eutectic solvent from the bottom of the absorption tower back to the absorption tower. The method can improve the quality of the nitrogen trifluoride product, and the content of carbon tetrafluoride impurities in the nitrogen trifluoride product can be reduced to 5 ppm, and the cost is low.

Provided is a plasma processing method capable of achieving flat etching process while suppressing vertical etching.The plasma processing method for plasma-etching a titanium nitride (TiN) film that forms a metal gate and contacts an insulating film on both sides includes the step of etching the titanium nitride (TiN) film by using plasmas that are generated by using a mixed gas of boron trichloride (BCl3) gas, nitrogen (N2) gas, and nitrogen trifluoride (NF3) gas and are generated by radio-frequency power modulated by a pulse, wherein the pulse has a first period with a first amplitude as its amplitude and a second period with a second amplitude as its amplitude and wherein the second amplitude is greater than 0 and less than the first amplitude.

The invention discloses a method for adsorbing and purifying nitrogen trifluoride gas, and relates to the technical field of nitrogen trifluoride adsorption and purification. The method for adsorbing and purifying nitrogen trifluoride gas comprises the following steps: uniformly mixing a 3A molecular sieve, a modifier and absolute ethyl alcohol, and heating for reaction to obtain an adsorbent; the method comprises the following steps: filling an adsorbent into an adsorption device, heating and activating in a nitrogen atmosphere, cooling to room temperature, and adsorbing a nitrogen trifluoride crude product through the adsorption device filled with the adsorbent under the conditions that the temperature is-25 to 10 DEG C, the pressure is 0.1 to 0.5 MPa and the flow is 0.25 to 0.70 m < 3 > / h, so as to obtain the HF-removed nitrogen trifluoride. According to the method for adsorbing and purifying the nitrogen trifluoride gas, the acidity of HF can be effectively reduced, and the used adsorbent has excellent compressive strength.

The invention relates to a method and a device for separating and refining nitrogen trifluoride and carbon tetrafluoride. The crude nitrogen trifluoride gas enters an adsorber in an adsorption state, an adsorbent selectively adsorbs carbon tetrafluoride, and a high-purity nitrogen trifluoride product is obtained at an outlet; meanwhile, hot inert gas is utilized to purge the adsorber in a desorption state, outlet regenerated gas enters a compressor after being cooled, and the regenerated gas enters a membrane separation assembly after being compressed; carbon tetrafluoride is used as permeation gas to permeate through the separation membrane, and residual waste gas is discharged to an incinerator. Main equipment comprises an adsorber in an adsorption state, an adsorber in a desorption state, a regeneration gas heater, a regeneration gas cooler, a compressor, a membrane separation assembly and the like. According to the method, nitrogen trifluoride and carbon tetrafluoride are separated through temperature swing and pressure swing adsorption, carbon tetrafluoride is efficiently and selectively adsorbed through the adsorbent to obtain the high-purity nitrogen trifluoride product, carbon tetrafluoride is separated and recycled through the membrane separation assembly, and the method has the advantages of being high in product purity and yield, low in cost and simple in process.

The invention discloses a production method of high-purity fluorine-nitrogen mixed gas, and belongs to the technical field of fluorine chemical industry. The method comprises the following steps: mixing high-purity nitrogen trifluoride and high-purity nitrogen according to a molar ratio of 1: (5.5-10), introducing the mixture into a cracker, reacting at the reaction temperature of 1000-1250 DEG C under the pressure of 0.2-0.7 Mpa until the pressure is not changed any more, cooling the reacted gas through a condenser, introducing the cooled gas into a buffer tank 1, compressing the cooled gas through a compressor, introducing the compressed gas into a de-heavy rectifying tower to remove heavy component impurities, and recovering the heavy component impurities to obtain the high-purity nitrogen trifluoride. And gas extracted from the top of the rectifying tower is introduced into the buffer tank 2, compressed by the compressor and then filled into a steel cylinder. The nitrogen is introduced into the cracking reaction, so that the safety of the reaction can be ensured, meanwhile, the production links of purifying fluorine gas and removing nitrogen impurities after the nitrogen trifluoride is cracked are reduced, the fluorine-nitrogen mixed gas with the preset concentration can be directly produced, the production cost is reduced, the production links are reduced, and the 20% fluorine-nitrogen mixed gas can be directly prepared.

To provide a substrate processing method and a substrate processing apparatus that selectively etch silicon oxide films without using hydrogen fluoride.SOLUTION: A substrate processing method includes a reaction step of heating a mixed gas of a reducing gas and nitrogen trifluoride to obtain an etching gas, and an etching step of bringing the etching gas into contact with a substrate having a silicon oxide film.SELECTED DRAWING: None

The invention provides a catalyst for nitrogen trifluoride decomposition and a preparation method thereof, and a decomposer, the catalyst comprises a bearing table and a catalyst layer; the bearing table is of a porous structure; the catalyst layer comprises a carrier and an active component, the active component is loaded on the carrier to form catalyst particles with the particle size being smaller than 100 nm, and the surface of the porous structure is coated with the catalyst particles to form the catalyst layer; wherein the carrier is doped with a transition metal oxide or a rare earth metal oxide; and the active component is a noble metal bimetallic composite material. According to the catalytic layer provided by the invention, the hydrogen fluoride corrosion resistance of the carrier is improved by adopting the transition metal oxide or the rare earth metal oxide, and the decomposition rate of nitrogen trifluoride on the surface of the catalytic layer is promoted and the reaction temperature of complete decomposition of nitrogen trifluoride is reduced by utilizing the effect of a noble metal bimetallic composite material, so that the catalytic activity is ensured.

The invention relates to methods for processing ammonium polyfluoride and producing nitrogen trifluoride (NF3). The technical result is the creation of a comprehensive, low-waste, explosion-proof technology for producing nitrogen trifluoride and, additionally, a group of inorganic fluorides: nitrogen trifluoride, carbon tetrafluoride, carbonyl fluoride, hydrogen fluoride and hydrofluoric acid. The proposed method envisages removing excess liquid ammonium polyfluoride from a reactor and sending it to be flaked or reacting it with oxygen, or with oxygen and carbon, or with oxygen and hydrogen-containing substances, or with oxygen and carbon and hydrogen-containing substances, or with fluorine, or with fluorine and hydrogen-containing substances, and recovering low-boiling substances by distillation and isolating hydrogen fluoride or hydrofluoric acid.

This invention relates to the field of additive manufacturing technology and discloses a method for preparing core-shell structured high-nitrogen steel composite powder for additive manufacturing. The method includes the following steps: hydrogen reduction treatment of high-nitrogen steel powder to remove the surface oxide film, obtaining reduced powder; nitrogen trifluoride activation treatment of the reduced powder to form nitride nuclei on the powder surface, obtaining activated powder; and ammonia nitriding treatment of the activated powder to grow the nitride nuclei into a dense nitride shell, obtaining core-shell structured high-nitrogen steel composite powder. This invention utilizes the synergistic effect of hydrogen reduction and nitrogen trifluoride activation to provide a highly active surface and uniform nucleation sites for ammonia nitriding, resulting in a dense nitride shell covering the powder surface. The obtained powder has a nitrogen content of 1.68%–2.29% and a Hall flow rate of 5.7 s / 50 g–6.5 s / 50 g. When this powder is used in selective laser melting additive manufacturing, the nitrogen retention efficiency reaches 78%~89%, the tensile strength of the printed parts is 782MPa~898MPa, and the elongation after fracture is 18.8%~32.1%.

There is provided a method for producing trifluoroamine oxide. The method includes a step of preparing an intermediate product by simultaneously providing and reacting nitrogen trifluoride and nitrous oxide under the presence of a SbF5 reaction activator; and a step of producing trifluoroamine oxide by reacting the intermediate product with potassium fluoride. The step of reacting the intermediate product with potassium fluoride is performed under atmospheric pressure and room temperature.

The application discloses a production method of high-purity fluorine-nitrogen mixed gas and belongs to the technical field of fluorine chemical industry. The method is characterized by mixing high-purity nitrogen trifluoride and high-purity nitrogen gas according to a 1:5.5-10 molar ratio, introducing the mixture into a cracking device, setting the reaction temperature to 1000-1250 DEG C, setting the pressure to 0.2-0.7 Mpa, reacting until the pressure does not change any more, cooling the reacted gas by a condenser and introducing the gas into a buffer tank 1, compressing the gas by a compressor, removing heavy component impurities in a heavy-removing rectifying tower, introducing the gas collected from the top of the rectifying tower into a buffer tank 2, compressing the gas by a compressor and filling the gas into a steel cylinder. The method can ensure the safety of the reaction, reduce the production steps of fluorine gas purification and nitrogen impurity removal after cracking of the nitrogen trifluoride, directly produce fluorine-nitrogen mixed gas with a predetermined concentration, reduce the production cost, reduce the production steps and directly prepare 20% fluorine-nitrogen mixed gas.

A vacuum processing method is provided that can prevent foreign matter from adhering to a wafer due to titanium (Ti)-based reaction products. The vacuum processing method can be applied to a plasma processing apparatus comprising: a sample stage disposed within a processing chamber within a vacuum container and holding a wafer having a titanium (Ti) film; a coil supplied with high-frequency power for forming plasma within the processing chamber; and a heating device that radiates electromagnetic waves to heat the wafer placed on the upper surface of the sample stage. The vacuum processing method includes the steps of etching the titanium (Ti) film and cleaning the processing chamber using a mixture of nitrogen trifluoride (NF3) gas, argon gas, and chlorine gas.

The invention relates to an electrolysis process system for preparing nitrogen trifluoride by electrolyzing ammonium bifluoride molten salt. The electrolysis process system comprises an electrolytic bath, a high-frequency switch direct-current power supply system, a hydrogen fluoride and ammonia gas feeding system, a cathode gas system and an anode gas system, the electrolytic bath comprises a bath body, a bath cover, cathodes and anodes, the bath cover is located above the bath body, the anodes and the cathodes are hung on the bath cover, fluoroplastic skirts or monel metal skirts are arranged between the cathodes and the anodes, and the cathodes and the anodes are arranged into a plurality of groups; the high-frequency switch direct-current power supply system is used for controlling current and voltage in the process of preparing nitrogen trifluoride by electrolysis of the electrolytic tank; the hydrogen fluoride and ammonia gas feeding system is used for conveying purified liquid hydrogen fluoride and high-purity ammonia gas into a tank body of the electrolytic tank and is interlocked with the liquid level of the electrolytic tank to realize automatic material supplementing; and the cathode gas system and the anode gas system are used for pretreating gases generated by a cathode and an anode in electrolysis. Safe and stable operation of production can be guaranteed, the labor intensity of operators is reduced, and the operation automation level is improved.

1. The name of the design product: remote plasma source emitter. 2. The use of the design product: used for dissociating nitrogen trifluoride gas into fluoride ion pairs for chamber cleaning, surface treatment, material modification, thin film deposition and other processes in a vacuum environment. 3. The design points of the design product: in shape. 4. The picture or photo that best indicates the design points: Design 1 perspective view. 5. Design 1 is designated as the basic design.

The utility model relates to the field of high-purity gas recycling, in particular to a reusable high-purity helium recovery device. Comprising a pneumatic diaphragm valve, a filter, a recovery tank, a one-way reciprocating pump and a helium tank which are arranged along the flow direction of high-purity helium, the pneumatic diaphragm valve is used for controlling the pressure of the recovery tank; the filter is used for filtering solid particles in high-purity helium; the recovery tank is used for recovering high-purity helium, and the one-way reciprocating pump is used for compressing and pressurizing the high-purity helium in the recovery tank and filling the high-purity helium into a helium bottle. According to the nitrogen trifluoride production pipeline recycling device, the recycling device capable of recycling the high-purity helium is connected in the nitrogen trifluoride production pipeline, waste of the high-purity helium is reduced through repeated use, the production cost requirement can be lowered, the cleanliness of the production pipeline can be guaranteed through the recycled high-purity helium, and the production quality is improved.

The utility model relates to a system for recovering HF (Hydrogen Fluoride) in nitrogen trifluoride electrolyte batching and storage emptying tail gas. A buffer tank, a condensing tower, an absorption tower, a water washing tower and an alkaline washing tower are sequentially connected through pipelines; the top of the buffer tank is connected with the middle part of the condensing tower; the bottom of the condensing tower is connected with a hydrogen fluoride collecting tank; the bottom of the absorption tower is connected with an absorption liquid storage tank, the outlet end of the absorption liquid storage tank is connected with a first circulating pump, and the outlet of the first circulating pump is respectively connected with an absorption tower spray head and an ammonium bifluoride crystallization kettle; the top of the water scrubber is connected with the middle of the alkaline tower, the bottom of the water scrubber is connected with a second circulating pump, and an outlet of the second circulating pump is respectively connected with the absorption tower spray header and the water scrubber spray header; the bottom of the alkaline tower is connected with a third circulating pump; an outlet of the third circulating pump is connected with an alkaline tower spray head. The system is simple in process and high in recovery economic value.

The invention provides a lithium battery electrolyte as well as a preparation method and application thereof. The lithium battery electrolyte is prepared from the following raw materials: thionyl chloride, lithium tetrachloroaluminate, sulfur dioxide and nitrogen trifluoride. Nitrogen trifluoride is added into the electrolyte, the nitrogen trifluoride reacts with a metal lithium negative electrode to generate a lithium fluoride enriched solid electrolyte interface with high ionic conductivity on the surface of the electrode in situ, so that the lithium ion transmission efficiency is remarkably improved, and the voltage hysteresis phenomenon is effectively improved. The preparation method is simple in process and remarkable in effect, and a new solution is provided for development of high-performance lithium thionyl chloride batteries.

The utility model discloses an energy-saving efficient evaporation system for nitrogen trifluoride production sewage. The energy-saving efficient evaporation system comprises a potassium fluoride waste liquid treatment unit, a sodium sulfate waste liquid treatment unit, a calcium chloride waste liquid treatment unit, a salt-rich water waste liquid treatment unit, a crystal evaporation separation unit, a crystal collection unit and a backwashing unit. The system disclosed by the utility model is used for separately treating four kinds of sewage, namely potassium fluoride waste liquid, sodium sulfate waste liquid, calcium chloride waste liquid and salt-rich water waste liquid generated in a nitrogen trifluoride production process to obtain multiple crystal products with single components, so that hazardous wastes and solid wastes are separately recycled, and the quantity of hazardous waste products and the treatment cost are reduced; one set of evaporation system is shared for intermittent treatment, so that the product production cost is reduced, the energy is saved, the consumption is reduced, the equipment production allowance is reasonably used, and the equipment utilization rate is improved.

An apparatus includes a body configured to support a substrate, a first coating, conformal on a surface of the body, that is corrosion resistant to at least one of: boron trichloride, nitrogen trifluoride, hafnium tetrachloride, aluminum trichloride, oxygen gas, chlorine gas, fluorine gas, chlorine trifluoride, hydrogen fluoride, hydrogen gas, ammonia, tungsten hexafluoride, tetrafluoromethane, titanium tetrachloride, molybdenum pentachloride, ozone, tetrafluorosilane, or hexafluoroethane, and a second coating, on the first coating, having a hardness that greater than or equal to about 8 gigapascals.

The application discloses a gas chromatography valve path system for analyzing the content of nitrogen trifluoride gas in carbon tetrafluoride and a use method thereof, and comprises one ten-way valve, one quantitative ring, three chromatographic columns and one detector, and comprises the following steps: (1) setting a valve event 0 min on the gas chromatography workstation, the state of the ten-way valve is "off", and carbon tetrafluoride sample gas enters a recovery pipeline; (2) setting a valve event 5 min on the gas chromatography workstation, the ten-way valve is "on", and the carbon tetrafluoride sample gas can enter the detector to analyze the peak. The method solves the problems of great operation difficulty, inaccurate measurement, and incomplete separation of the main component carbon tetrafluoride and the impurity component nitrogen trifluoride in the prior art, the valve path system is clear, the operation is simple and convenient, and the analysis is accurate.

The invention relates to a method and a device for purifying crude nitrogen trifluoride gas, and belongs to the technical field of nitrogen trifluoride gas purification, and the method comprises the following steps: sequentially carrying out preheating, cracking, hydrogen fluoride washing, reduction, alkali washing, water ring pressurization, water removal and secondary rectification on nitrogen trifluoride electrolytic gas prepared by adopting an electrolytic method. According to the method, the high-purity nitrogen trifluoride gas with the purity of 99.995 vol% or above can be obtained, and the method is safe to operate, low in cooling medium consumption and low in energy consumption; the device comprises a preheater, a cracking tower, a buffer tank, a hydrogen fluoride washing tower, a reduction tower, an alkaline washing tower, a water ring compressor, water removal equipment, a rectification system and a filling system, and the method and the device are simple in structure, high in operation safety, strong in operability, low in operation cost, suitable for large-scale production and wide in application prospect.

1. Name of the product in this design: Remote Plasma Source Power Supply (45L). 2. Application of this design: It is used to provide power to a 45L remote plasma source chamber to dissociate nitrogen trifluoride gas into fluoride ions for chamber cleaning, surface treatment, material modification, thin film deposition and other processes in a vacuum environment. 3. The key design feature of this product is its shape. 4. The image or photograph that best illustrates the design's key points: a 3D model.

The invention relates to a method for preparing a nickel-iron-carbon catalyst from nickel slag solid waste, which comprises the following steps: S1, dissolving nickel slag generated in the process of electrolyzing nitrogen trifluoride in dilute nitric acid to prepare a mixed solution; s2, adding polyacrylamide into the mixed solution, and fully stirring; s3, adding a concentrated alkali solution into the fully stirred solution until the solution is alkaline, filtering the solution, and freeze-drying the obtained solid precipitate; and S4, carrying out high-temperature calcination on the dried solid mixture under an anaerobic condition, naturally cooling to room temperature, and sequentially washing with water and absolute ethyl alcohol to obtain the final nickel-iron-carbon catalyst. The nickel-iron-carbon catalyst is used for catalyzing potassium hydrogen persulfate to degrade bisphenol A in wastewater. The catalyst prepared by the method has excellent catalytic performance and stability.

An ammonium fluoride gas may be used to form a protection layer for one or more interlayer dielectric layers, one or more insulating caps, and / or one or more source / drain regions of a semiconductor device during a pre-clean etch process. The protection layer can be formed through an oversupply of nitrogen trifluoride during the pre-clean etch process. The oversupply of nitrogen trifluoride causes an increased formation of ammonium fluoride, which coats the interlayer dielectric layer(s), the insulating cap(s), and / or the source / drain region(s) with a thick protection layer. The protection layer protects the interlayer dielectric layer(s), the insulating cap(s), and / or the source / drain region(s) during the pre-clean process from being etched by fluorine ions formed during the pre-clean process.

The invention provides a treatment method for nickel-containing waste residues generated in the process of preparing nitrogen trifluoride through an electrolytic method. According to the method, separation and recovery of metal iron and nickel in nickel residues are achieved through fractional precipitation; the technological process is simple, the added materials are non-toxic and harmless, and introduction of ammonia gas is avoided in the nickel recovery process; wastewater generated in the system can be recycled; metal iron and nickel can be efficiently recycled, and a high-value nickel hydroxide product and a high-value ferric hydroxide byproduct are obtained; secondary pollution is avoided, the operation cost is low, and obvious economic benefits and environmental benefits are achieved.

The application discloses a method for adsorbing and purifying nitrogen trifluoride gas and relates to the technical field of nitrogen trifluoride adsorption and purification. The method comprises the following steps: uniformly mixing 3A molecular sieve, a modifier and anhydrous ethanol, and performing a temperature rising reaction to obtain an adsorbent; the adsorbent is filled into an adsorption device, activated under a nitrogen atmosphere, and then cooled to room temperature; crude nitrogen trifluoride is subjected to adsorption in the adsorption device filled with the adsorbent under the conditions that the temperature is-25-10 DEG C, the pressure is 0.1-0.5 MPa, and the flow rate is 0.25-0.70 m 3 / h, and nitrogen trifluoride from which HF is removed is obtained. The method can effectively reduce the acidity of HF, and the adsorbent used has excellent compressive strength.