22results about "Tungsten halides" patented technology

The invention discloses a synthesis process of tungsten hexafluoride, and relates to the technical field of special gas synthesis. The process comprises the following steps: mixing ammonium fluoride and hydrofluoric acid to prepare an activation solution, carrying out ultrasonic activation treatment on tungsten powder to obtain pretreated tungsten powder, and reacting the pretreated tungsten powder with fluorine gas at a certain temperature and pressure to prepare a liquefied crude product tungsten hexafluoride; the preparation method comprises the following steps: by taking aluminum sec-butoxide and the like as raw materials, carrying out sol-gel and ethanol supercritical drying and calcining to prepare highly porous activated aluminum oxide; gasifying the crude tungsten hexafluoride, adsorbing with activated aluminum oxide, and rectifying to obtain purified tungsten hexafluoride liquid; and finally, dissolving in liquid sulfur dioxide, treating under illumination with the wavelength of 395nm, and carrying out distillation separation to obtain high-purity tungsten hexafluoride. According to the method, the activation pretreatment is combined with multi-stage purification, so that the purity and the synthesis efficiency of tungsten hexafluoride are remarkably improved.

This invention discloses a process for preparing chlorides by reducing chlorination with rare metal oxides, comprising the following steps: S1, in an inert atmosphere, a mixture containing rare metal oxide powder, a reducing agent, and a chloride salt is subjected to a reduction reaction at a predetermined temperature 1; S2, the temperature is lowered to a predetermined temperature 2, oxygen is introduced, and the concentration of oxygen in the mixed gas is adjusted to carry out a chlorination reaction, and the chlorinated product is condensed and collected. This invention eliminates the need for gaseous chlorinating agents such as chlorine or hydrogen chloride, avoiding the leakage risks of liquid chlorine and compressed hydrogen chloride during storage and transportation; the raw materials can be directly rare metal oxides, with a wide range of sources, good process adaptability, and significantly reduced production costs.

The invention relates to the technical field of chemical engineering, in particular to a preparation method of tungsten pentachloride, which comprises the following steps: S1, feeding tungsten hexachloride into a fluidized bed reactor through gravity and inert gas flow, continuously introducing inert gas into the fluidized bed reactor, keeping the tungsten hexachloride in the fluidized bed reactor to be fluidized, preheating and preserving heat; s2, introducing mixed gas of nitrogen or inert gas and hydrogen into the fluidized bed reactor, and reacting in the fluidized bed reactor; and S3, collecting tungsten pentachloride. The equipment and operation are simple, continuous production of high-quality tungsten pentachloride can be achieved, the technological process is simple, the operation unit is small, daily operation and maintenance are simple, and automatic control is facilitated.

High purity tungsten precursors and methods for purifying the tungsten precursors are provided. The method for purifying the precursors can include at least one of the following steps: obtaining a source container containing WCl4, WOCl4, and either WCl5 or WCl6, separating the WCl5 or WCl6 from at least a first portion of the WOCl4, separating the WCl5 or WCl6 from at least a second portion of the WOCl4, collecting the precursors in a collection container, or any combination thereof.

A device which can be exposed to chemical vapors, such as a molybdenum vapor, a tungsten vapor, or any combination thereof, which has a coating covering at least a portion thereof. The coating reduces or inhibits mass change at an outer surface of the device from exposure to the vapor. In certain situations, the mass change is a mass gain, and the coating reduces or inhibits the mass gain of equal to or less than 1 x 10-5 g mm-2.

A method for removing fluorine gas from a fluorine-containing gas containing fluorine gas and a fluorine-containing compound gas is provided. A method for removing fluorine gas from a fluorine-containing gas containing fluorine gas and a fluorine-containing compound gas includes a removal step in which the fluorine-containing gas is brought into contact with at least one metal salt selected from the group consisting of metal chlorides, metal bromides, and metal iodides.

The precursor includes a tungsten precursor and a carbon-containing material. The precursor includes less than 0.02 wt.% of the carbon-containing material, based on the total weight of the precursor. A method for purifying a tungsten precursor can include at least one of obtaining a source container including the tungsten precursor and the carbon-containing material, separating the tungsten precursor from at least a first portion of the carbon-containing material, recovering the precursor in a collection container, or any combination thereof.

The application discloses a preparation method of rare metal chloride, which comprises the following steps: in an inert atmosphere, a mixture containing rare metal powder, a chlorine salt and an auxiliary material is heated to a predetermined temperature, oxygen is introduced, the concentration of oxygen in the mixed gas is adjusted, a chlorination reaction is carried out, and a chlorination product is condensed and collected to obtain the rare metal chloride. The application avoids the safety production risk caused by the use of chlorine or hydrogen chloride in the traditional production, and the production process avoids the leakage risk of liquid chlorine and compressed hydrogen chloride in the storage and transportation process. Since the reaction process is a double decomposition reaction, the reaction rate is controllable, the reaction does not have obvious heat release, and is safe and reliable. The chlorine content in the production tail gas is extremely low, and the environmental pollution problem caused by a large amount of chlorine-containing tail gas in the traditional chlorination process is avoided.

Compositions are provided. A composition comprises a tungsten pentachloride compound. The tungsten pentachloride compound has an orthorhombic crystal structure as determined using Single-Crystal X-ray Diffraction. A method comprises obtaining a precursor, vaporizing the precursor to obtain a vaporized precursor, and exposing, under vapor deposition conditions, a substrate to the vaporized precursor. The precursor comprises a tungsten pentachloride compound having an orthorhombic crystal structure as determined by Single-Crystal X-Ray Diffraction. Related precursors and related methods are also provided, among other things.

The present application relates to a kind of hydrogen removal nonmetallic impurities in tungsten hexafluoride system, including primary light removal tower, the primary light removal tower outlet is communicated secondary light removal tower, the primary light removal tower and secondary light removal tower top outlet is communicated light component tank, the secondary light removal tower outlet is communicated column tube heat exchanger, the column tube heat exchanger is communicated collector;The present application also relates to a kind of hydrogen removal nonmetallic impurities in tungsten hexafluoride method, from the bottom of primary light removal tower, crude tungsten hexafluoride with hydrogen is introduced, and it is carried out under high temperature, catalyst condition oxidation reduction;After oxidation reduction, into secondary light removal tower, it is further reduced under higher temperature, form mixed gas, unreacted hydrogen and light component from the top of secondary light removal tower into light component tank;Mixed gas is collected after heat exchange, finally complete the removal of nonmetallic impurities in tungsten hexafluoride.The present application realizes the continuous operation of tungsten hexafluoride purification, process operation is simple, and reaction efficiency is high.

The present invention relates to a process for the co-production of tungsten halides and carbon tetrafluoride. Tungsten carbide or a mixture of tungsten carbide and carbon is added to a reactor, chlorine trifluoride gas is introduced into the reactor, the reactor temperature is controlled at 340-400°C, the reaction pressure is 0.01-0.15 MPa, and a reaction is carried out to obtain a mixture comprising tungsten hexachloride, tungsten pentachloride, tungsten hexafluoride, and carbon tetrafluoride. After the reaction is completed, the reaction products are sequentially collected through a four-stage cold trap, with the first stage collecting tungsten hexachloride, the second stage collecting tungsten pentachloride, the third stage collecting tungsten hexafluoride, and the fourth stage collecting carbon tetrafluoride. The present invention has relatively mild reaction conditions, a reaction temperature below 400°C, higher safety, low raw material cost, high atom economy, higher safety, lower energy consumption, no by-products, and great economic benefits and development prospects. It meets the production requirements of chemical enterprises for safety, environmental protection, high efficiency, and circular economy.

Compositions are provided. A composition comprises a tungsten pentachloride compound. The tungsten pentachloride compound has an orthorhombic crystal structure as determined using Single-Crystal X-ray Diffraction. A method comprises obtaining a precursor, vaporizing the precursor to obtain a vaporized precursor, and exposing, under vapor deposition conditions, a substrate to the vaporized precursor. The precursor comprises a tungsten pentachloride compound having an orthorhombic crystal structure as determined by Single-Crystal X-Ray Diffraction. Related precursors and related methods are also provided, among other things.

Methods for synthesizing and / or purifying molybdenum compounds are provided. A method comprises obtaining a reagent; obtaining a metal trioxide compound; and contacting the reagent and the metal trioxide compound sufficient to form a reaction product comprising a molybdenum compound. Related compositions, related systems, and other related methods are provided, among other things.

This application provides a method for preparing metal chlorides. This method and apparatus solve the problem of inaccurate flow metering of chlorides as reactants in existing chemical vapor deposition (CVD) processes. The method includes: installing a dedicated chlorine flow meter at the inlet of a chlorine gas inlet pipe; adding bulk metal to a reaction vessel and sealing the vessel; purging the reaction vessel containing the bulk metal with an inert protective gas, heating to remove water and oxygen; heating to a specified temperature, shutting off the inert protective gas, and starting the chlorine gas reaction. This invention precisely controls the flow rate of the chlorine gas to generate a fixed amount of metal chloride. Under the action of a reducing gas, a uniformly deposited, high-strength metal / carbide coating is obtained on the substrate surface. This coating is virtually free of impurities, and the deposited substrate can be used in industries such as semiconductors and medicine. This method is low-cost, produces stable products, and is easy to scale up.

Methods and related systems are provided for removing impurities from a precursor. A method includes at least one thermal cycle. The at least one thermal cycle includes one or more of the following steps: heating a vessel including a precursor and at least one impurity to a temperature for a duration sufficient to vaporize at least a portion of the at least one impurity; measuring a vapor pressure within the vessel to obtain a measured vapor pressure and comparing the measured vapor pressure to a set vapor pressure; and removing at least a portion of the vapor including the at least one impurity from the vessel when the measured vapor pressure is higher than or within the setpoint vapor pressure. Other methods and systems are provided herein.

The present application relates to a kind of system for processing tungsten hexafluoride synthesis tail gas, including intake pipeline;The one end of the intake pipeline is communicated with tungsten hexafluoride synthesis tail gas discharge pipe, and the other end of the intake pipeline is divided into two-way pipeline, and two-way pipeline is connected adsorption tower A and adsorption tower B respectively, and the adsorption tower A and adsorption tower B are arranged in parallel, and the top of the adsorption tower A and adsorption tower B is connected waste gas absorption tower, and the bottom of the adsorption tower A and adsorption tower B is connected plasma reactor, and the outlet of the plasma reactor is connected product collection tank.The present application relates to a kind of method for processing tungsten hexafluoride synthesis tail gas, including tail gas absorption and adsorption tower regeneration step.The present application realizes trace NF3 and high-purity tungsten powder reaction, further recovers NF3 in tail gas, reduces WF6 production cost and tail gas processing cost.

A precursor comprises a tungsten precursor and a carbon-containing material. The precursor comprises less than 0.02% by weight of the carbon-containing material based on a total weight of the precursor. A method for purifying a tungsten precursor may comprise at least one of the following steps: obtaining a source vessel containing a tungsten precursor and a carbon-containing material; separating the tungsten precursor from at least a first portion of the carbon-containing material; recovering a precursor in a collection vessel; or any combination thereof.

Removing metal from metal-carbon material includes contacting the metal-carbon material with hydrogen chloride, thereby yielding a metal chloride in the gas phase and a solid product comprising carbon. The metal-carbon material and the solid product may both contain elemental carbon. A concentration of metal in the solid product is typically less than 1 wt%.

Methods for synthesizing and / or purifying molybdenum compounds are provided. A method comprises obtaining a reagent; obtaining a metal trioxide compound; and contacting the reagent and the metal trioxide compound sufficient to form a reaction product comprising a molybdenum compound. Related compositions, related systems, and other related methods are provided, among other things.

The present invention discloses an electronic-grade tungsten hexafluoride purification device, comprising: a heating tube for heating a tungsten hexafluoride mixed gas to 150°C-400°C; a buffer tank, one end of which is connected to the heating tube and the other end of which is provided with a connecting pipe; a reduction tower, the bottom of which is connected to the connecting pipe and the top of which is provided with an exhaust pipe; and a stuffing pipe, which is arranged in the reduction tower and has a breathable structure so that the tungsten hexafluoride mixed gas can only pass through the stuffing pipe and be discharged from the exhaust pipe. The stuffing pipe is filled with tungsten pellets and can automatically discharge used tungsten pellets and refill them with new tungsten pellets according to the intake volume of the tungsten hexafluoride mixed gas.

The application discloses a novel method and device for resource conversion of sulfur hexafluoride. The method comprises the following steps: firstly, performing primary discharge treatment on SF6 to dissociate SF6 into fluorine atoms and low-fluorine sulfides; secondly, performing fluorination reaction of the fluorine atoms and the low-fluorine sulfides with tungsten to convert the fluorine atoms and the low-fluorine sulfides into WF6 and reduce sulfur into elemental sulfur; thirdly, controlling the fluorination reaction temperature to be 120-160 DEG C to make the generated elemental sulfur into liquid state, so that the elemental sulfur is conveniently collected; fourthly, condensing mixed gas containing WF6, collecting the liquefied WF6, mixing the condensed mixed gas with water vapor, and performing secondary discharge treatment on the mixed gas containing water vapor; under the action of the water vapor, the mixed gas is further degraded, and the degradation products tend to be SO2 and HF; fifthly, separating the SO2 and the HF; sixthly, treating the HF by using a "hydrogen fluoride-liquid ammonia" liquid phase method to obtain ammonium fluoride and ammonium bifluoride; and seventhly, treating the SO2 by using a wet ammonia method to obtain ammonium sulfite and ammonium sulfate.

Tungsten precursors with high purity and methods for purifying tungsten precursors are provided. The method for purifying a precursor may comprise at least one of the following steps: obtaining a source vessel containing WCl4, WOCl4, and one of WCl5 or WCl6; separating the WCl5 or the WCl6 from at least a first portion of the WOCl4; separating the WCl5 or the WCl6 from at least a second portion of the WOCl4; recovering a precursor in a collection vessel; or any combination thereof.