38 results about "Tungsten hexacarbonyl" patented technology

The invention discloses a plasma-type tungsten oxide-modified graphite phase carbon nitride nanosheet composite photocatalyst and a preparation method and application thereof. The composite photocatalyst comprises a plasma-type tungsten oxide and a graphite phase carbon nitride nanosheet. The plasma-type tungsten oxide attaches to the surface of the graphite phase carbon nitride nanosheet. The plasma-type tungsten oxide is W18O49. The preparation method comprises mixing the graphite phase carbon nitride nanosheet and a tungsten hexacarbonyl solution to obtain a precursor mixed solution and preparing a composite photocatalyst through a hydrothermal reaction. The composite photocatalyst has the advantages of high photocatalytic activity, wide photoresponse range, stable photocatalytic performance and good recyclability. The preparation method has the advantages of simple processes, operation easiness and low cost. The composite photocatalyst can be used for treating antibiotic waste water, can be used through a simple method, realizes a low cost, has a high removal rate, effectively degrades antibiotics in waste water and has a good application prospect.

The invention discloses a manufacturing method for a pure tungsten or molybdenum thin-wall device, belonging to the technical field of powder metallurgy. The manufacturing method comprises the following process steps of: manufacturing a template of the required device by using a red copper material and keeping the surface clean and dry, wherein the surface roughness Ra of the template is lower than 6.3; placing the template into a vapor deposition chamber; with tungsten hexacarbonyl or molybdenum hexacarbonyl as an reactive organic source and with high-purity hydrogen gas or nitrogen gas as diluent gas, carrying out thermal decomposition vapor deposition on the template under the conditions that the pressure of the vapor deposition chamber is 500-10000Pa and the deposition temperature is 280-420DEG C and carrying out annealing once every 2-4 hours in the deposition process according to the requirement of the deposited wall thickness; after the deposition is finished, closing an organic source valve and continuously introducing the dilute gas and keeping the device cooled to the room temperature; and removing a red copper template matrix from the device of which the template surface is deposited with tungsten or molybdenum by adopting a nitric acid corrosion method to obtain the pure tungsten or molybdenum thin-wall device with the wall thickness being 0.1-3mm. The manufacturing method has the advantages of low deposition temperature, high deposition speed, high purity of deposition film, dense film layer, favorable smoothness of film surface, short process flow and no pollution or corrosion.

The invention provides a preparation method of a palladium-copper bimetallic nanoflower peroxide. The preparation method comprises the following steps: adding sodium tetrachloropalladate, tungsten hexacarbonyl, copper chloride dihydrate, dimethylformamide and glacial acetic acid to a round-bottom flask; ultrasonically and uniformly mixing the above solutions, and then heating and stirring the uniformly mixed solutions through an oil bath; and finally, centrifugally washing the obtained product by using water and ethanol for serval times, so as to obtain a bimetallic alloy nanomaterial, namelyPdCu nanoflower. The preparation process of the palladium-copper bimetallic nanoflower peroxide is simple and the yield is high; and through the prepared unique two-dimensional structure, the reactionrate is promoted and the detection time is saved. The invention further discloses the application of the palladium-copper bimetallic nanoflower peroxide to glucose detection. Through such a detectionmethod, the sensitivity and the selective detection of glucose can be achieved.

The invention discloses a preparation method of ultra-fine tungsten carbide powder and belongs to the technical field of powder metallurgy. The preparation method of the ultra-fine tungsten carbide powder comprises the technological steps that 100 mass parts of tungsten hexacarbonyl W(CO)6 and 3-5 mass parts of dicobalt octacarbonyl Co2(CO)8 are dissolved in diethyl ether in a three-opening bottle and stirred to be completely dissolved, and the diethyl ether is evaporated through vacuum distillation, so that a solid uniform mixture of the ungsten hexacarbonyl W(CO)6 and the dicobalt octacarbonyl Co2(CO)8 is obtained; the three-opening bottle is heated to the temperature of 50-90 DEG C, carrier gas is introduced to carry the gasified W(CO)6 mixture into a pyrolyzing furnace, methane gas preheated to the temperature of 300-450 DEG C is introduced into the pyrolyzing furnace at the same time, the temperature of the pyrolyzing furnace is kept being 300-450 DEG C, and the reaction time is 30-120 minutes; and the ultra-fine tungsten carbide powder which contains 1.0%-6.5% of cobalt by mass is finally obtained, and the granularity D50 of the powder is 50-600 nm. By the adoption of the method, the granularity of the tungsten carbide powder can be controlled; in addition, due to the fact that the tungsten carbide powder is doped with certain cobalt, abnormal growth of the tungsten carbide powder during high-temperature sintering can be restrained, and the excellent performance of the tungsten carbide powder is kept.

The invention relates to a method for directly synthesizing a metal (tungsten or molybdenum) carbonyl complex from tungsten oxide or molybdenum oxide, belonging to the technical field of powder metallurgy. The method comprises the following steps: putting tungsten or molybdenum oxide, carbon tetrachloride, a nonpolar organic solvent and an independently packaged reducer into a sealed reaction kettle provided with a stirrer; replacing air in the reaction system by repeatedly charging carbon monoxide into the reaction kettle and discharging the carbon monoxide from the reaction kettle, heating the reaction kettle to 200-250 DEG C, and keeping the temperature for 4-8 hours; after the reaction system is cooled to 30-50 DEG C, introducing carbon monoxide to 5-20 MPa, keeping the pressure, starting the stirrer of the reaction kettle, breaking the container packaging the reducer, wherein the stirring is carried out at the rotation speed of 100-200 rpm for 1-12 hours; and after the reaction finishes and the solution is cooled to room temperature, taking out the reaction solution, distilling and heating for sublimation to obtain the clear crystal of tungsten hexacarbonyl or molybdenum hexacarbonyl. The invention has the advantages of simple technique, high safety in production, low cost and high synthesis efficiency, and has wide application prospects in the market.

The invention discloses a synthesis method of a flower-like palladium oxide-gold nano composite material. The synthesis method comprises the following steps of (1) N, N-dimethylformamide, Pd (acac) 2,citric acid, hexadecyl trimethyl ammonium bromide and polyvinylpyrrolidone are selected, and uniformly mixing is conducted to obtain an orange red liquid; (2) tungsten hexacarbonyl is added into theorange red liquid, the temperature is adjusted in an argon atmosphere, and stirring reaction is carried out to obtain a blue hexagonal palladium nanosheet; (3) the blue hexagonal palladium nanosheet is purified by using a mixed solvent of acetone and ethanol to obtain purified palladium; and (4) the purified palladium is dissolved in ultrapure water to obtain a palladium nano solution, and the palladium nano solution and chloroauric acid are stirred and reacted to obtain the flower-like palladium oxide-gold nano composite material. The invention further discloses the flower-like palladium oxide-gold nano composite material synthesized by the method, application of the composite material as an active substrate in surface enhanced Raman scattering and application of the composite material inthe aspect of a photo-thermal effect.

The invention discloses a preparation method of a WS2/FeS nanosphere hybrid catalyst, which comprises the following steps: S101, dissolving tungsten hexacarbonyl and sulfur powder in an organic solvent under the protection of inert gas, uniformly mixing, dropwisely adding a certain amount of iron pentacarbonyl, and uniformly mixing at room temperature to obtain a brown mixed solution; S102, fullyreacting the brown mixed solution in a high-pressure reaction kettle at the temperature of 100 DEG C and 250 DEG C to obtain a mixture; preferably, the brown mixed solution is fully reacted for 10-24hours; and S103, cooling the reacted high-pressure reaction kettle to room temperature, centrifuging the mixture to obtain a black precipitate, and purifying the black precipitate to obtain the product. The invention provides the WS2/FeS nanosphere hybrid catalyst prepared by the method and an application of the WS2/FeS nanosphere hybrid catalyst. The preparation method of the WS2/FeS nanosphere hybrid catalyst is simple, and nanosheet cluster type nanoparticles with uniform size and high specific surface area are obtained.

The invention discloses a method for preparing tungsten diselenide nanotubes. The method comprises the following steps: 1) laying tungsten hexacarbonyl to the bottom of a ceramic crucible, laying a porous anodic aluminum oxide mold plate with an opening facing downwards on the tungsten hexacarbonyl, sealing the ceramic crucible, putting into a tubular furnace, performing low-temperature sublimation deposition in the presence of a gas, and continuously performing heating pyrolysis; 2) cooling the vacuum tubular furnace to the room temperature, putting the mold plate with the opening facing downwards into a ceramic crucible with selenium powder, sealing the ceramic crucible, heating in the presence of the gas, and enabling a single substance, namely selenium, to react with a metal, namely tungsten, directly; 3) removing the excessive aluminum oxide mold plate and excessive selenium by using a diluted acid solution, performing suction filtration treatment, and drying, thereby obtaining afinished product. The method disclosed by the invention is simple in step, free of environment pollution and free of complex equipment, a tungsten diselenide nanotube powder material prepared by usingthe method is good in size controllability, good in crystallinity and uniform in nanotube wall and morphology, and thus the comprehensive properties of a finished product of the tungsten diselenide nanotube powder material are greatly improved. The method is wide in applicability and beneficial to large-scale industrial production.

The invention relates to a flower-like palladium hydride catalyst for catalyzing oxygen reduction reaction. A preparation method for the flower-like palladium hydride catalyst comprises the following steps: respectively weighing 1-50 mg of sodium chloropalladate and tungsten hexacarbonyl, adding 1-20 mL of an N,N-dimethylformamide solution, fully mixing formed solutions, and then adding 1-10 mL of acetic acid solution; after the solutions in the previous step are fully mixed, putting the mixed solution into an oil bath pan, conducting heating to 50-200 DEG C, performing reacting for 1-10 hours, and successively carrying out washing, centrifuging and drying to obtain flower-shaped palladium; and weighing 1-10 mg of prepared flower-like palladium, adding 1-50 mL of the N,N-dimethylformamide solution, conducting uniform mixing, performing heating to 50-200 DEG C in the oil bath pan, carrying out reacting for 1-30 hours, and then successively carrying out washing, centrifuging and drying to obtain the flower-like palladium hydride catalyst. The invention also provides the preparation method of the catalyst. The preparation method is simple in process, and the prepared catalyst has excellent electrochemical oxidation-reduction performance.

The invention discloses a preparation method of a tungsten trioxide nanotube. The preparation method comprises the following technological steps: firstly, paving hexacarbonyl tungsten at the bottom ofa ceramic crucible, then downward putting an opening of a porous anodic alumina template above the hexacarbonyl tungsten, sealing the crucible, then putting the crucible into a tubular furnace for heating, and carrying out low-temperature sublimation to form deposited hexacarbonyl tungsten; continuously heating and pyrolyzing to form deposited metal tungsten; secondly, continuously heating and enabling the deposited hexacarbonyl tungsten in the first step to be deposited and oxidized; thirdly, removing the porous anodic alumina template by using a dilute acid solution, then carrying out suction filter treatment, and drying to obtain a finished product. The method disclosed by the invention has the advantages of simple steps, no environmental pollution and no need of complex equipment; theprepared tungsten trioxide nanotube powder material has the advantages of high size controllability, good crystallinity and uniform tube wall and morphology of the nanotube, thereby greatly improvingoverall performance of a finished product of the tungsten trioxide nanotube powder material. The preparation method disclosed by the invention has wide applicability and facilitates large-scale industrial production.

The invention belongs to the technical field of nanometer and particularly relates to a preparation method of tin nanoparticles and a lithium ion battery negative electrode material. The preparation method comprises steps that in an inert atmosphere, tin precursor, tungsten hexacarbonyl, oleylamine and hexamethyldisilazane are dissolved in non-coordination solvent to obtain mixture; the mixture issubjected to heating reaction, after the reaction is finished, reaction liquid is cooled to the room temperature and subjected to solid-liquid separation treatment, and the tin nanoparticles are obtained. The preparation method is advantaged in that tungsten hexacarbonyl is adopted as reducing agent, oleylamine and hexamethyldisilazane are adopted as ligands, the non-coordination solvent is adopted as reaction solvent, under the synergistic effect of all reaction raw material, the tin nanoparticles uniform in particle size and small in size are prepared, the particle size distribution is narrow, and the average particle size standard deviation is only 6%-8%. The method is advantaged in that the method is simple, operation is easy and convenient, all the reaction raw material substances are low in toxicity and high in efficiency, and large-scale production of the tin nanoparticles is easy.

The invention discloses a preparation method of a phosphorized WS2 nanosphere catalyst, which comprises the following steps of S101, dissolving tungsten hexacarbonyl and powdered sulfur in an organic solvent under the protection of inert gas, and uniformly mixing at room temperature to obtain a brown mixed solution, fully reacting the brown mixed solution in a high-pressure reaction kettle at 100-250 DEG C, wherein the brown mixed solution fully reacts for 10-24 hours, S102, cooling the high-pressure reaction kettle after the reaction to room temperature, centrifuging the mixture to obtain a black precipitate, and purifying, S103, enabling the purified black precipitate to react with sodium hypophosphite for 2-3 h at the temperature of 200-300 DEG C in a tubular furnace filled with inert gas, and then acquiring the product. The invention provides the WS2P nanosphere catalyst prepared by the method and application of the WS2P nanosphere catalyst. The preparation method of the WS2P nanosphere catalyst is simple, and nanosheet cluster type nanoparticles with uniform size and high specific surface area are obtained.

The present invention is directed to an alpha-W layer which is employed in interconnect structures such as trench capacitors or damascene wiring levels as a diffusion barrier layer. The alpha-W layer is a single phased material that is formed by a low temperature/pressure chemical vapor deposition process using tungsten hexacarbonyl, W(CO)₆, as the source material.

The invention discloses a method for synthesizing platinum-rhodium nanocrystals with small particle diameters. As the reaction raw materials, the above-mentioned reaction raw materials are added to the dimethylformamide solution one by one, and ultrasonically mixed to obtain a mixed solution; (2) The mixed solution is heated to 150-160 ° C at a heating rate of 5-10 degrees/min Keeping the temperature constant, reacting for 5-10 hours to obtain a black solution, then cooling, centrifuging and washing the product to obtain a platinum-rhodium nanocrystal product with a particle size of 2-5nm. The present invention is the first to prepare platinum-rhodium nanocrystal material. Due to the introduction of rhodium, the material enhances the ability to break the C-C bond, and strengthens the anti-poisoning ability to CO. The catalytic performance and stability of the material far exceed that of commercial platinum. / carbon, the potential practical value of the material is high.

The invention discloses a method for purifying high-purity tungsten hexacarbonyl, which comprises the following steps of: dewatering raw materials, namely dewatering tungsten hexacarbonyl in a manner of placing in a vacuum oven; carrying out sublimation in an oxygen-free anhydrous inert atmosphere, sublimating the raw materials by adopting a sublimation column, removing low-boiling-point fractions and high-boiling-point impurities, and collecting middle-section fractions; performing high-vacuum operation on the system, changing the vapor pressure of the system by adopting high vacuum, continuously changing the vacuum degree of the system, and separating low-boiling-point and high-boiling-point impurities; and scraping, and collecting high-purity tungsten hexacarbonyl. According to the present invention, with the purification method, the organic impurities in the tungsten hexacarbonyl can be effectively removed, the inorganic impurities in the tungsten hexacarbonyl can be removed through the ICP-OES full-element detection, the content of all the inorganic impurities is less than 1 ppm, and the purity of the tungsten hexacarbonyl obtained through the purification method is as high as 99.9999%, such that the raw material use requirements of the semiconductor industry can be met.

The invention discloses a preparation method for continuously growing a two-dimensional semiconductor tungsten selenide (WSe2) film through MOCVD. The preparation method comprises the following steps: cleaning a c-plane sapphire substrate; putting the cleaned substrate into an MOCVD reaction cavity, carrying out high-temperature pretreatment on the substrate, and depositing a WSe2 thin film on sapphire through MOCVD continuous growth by taking tungsten hexacarbonyl (W(CO)6) and hydrogen selenide (H2Se) as precursors; and annealing the WSe2 film growing on the sapphire to obtain a continuous and large-area finished product with high crystallization quality. The film annealing is carried out in a mixed atmosphere of hydrogen (H2) and argon (Ar) at the temperature of 200-400 DEG C for 2-3 hours, and the heating and cooling rate in the annealing treatment process is 40-60 DEG C/h. The method has the advantages that gas sources are adopted as precursors, and carbon pollution of powder is avoided; and the continuous, large-area, high-electrical-performance and controllable-growth WSe2 thin film can be obtained after 60-100 min, and has important application prospects in the field of microelectronics.

The invention discloses an electron beam divergence angle measuring device and a preparation method and a measuring method thereof. The device comprises a fluorescent screen and tungsten micro-nano patterns, tungsten hexacarbonyl is deposited on the fluorescent screen through a helium ion microscope to form the tungsten micro-nano patterns, the tungsten micro-nano patterns are a plurality of concentric circles, and the circle centers of the concentric circles are located in the center of the fluorescent screen. A tungsten micro-nano pattern is constructed on a fluorescent screen by utilizing ion-assisted deposition of a helium ion microscope, when the fluorescent screen is moved, the spot shape and the size of an electron beam hit on the fluorescent screen are changed, and an electron beamspot and an electron beam divergence angle are directly measured according to the size and the size of the tungsten micro-nano pattern. The device has the advantages of multiple functions, high measurement precision, simple operation and the like; the preparation method has the advantages of high precision, easiness in control, simple process and the like.