Producing chemoresistive organic vapor sensor by e.g. mixing powder of metallic niobium, graphite and aluminum carbide, placing mixture in crucible, transferring, heating, cooling, removing mixture, grinding and adding powder to reactor
2023-05-22
专利权人UNIV SARAT STATE TECH (UYSA-C)
申请日期2023-05-22
专利号RU2023113251-A; EA48111-B1
成果简介NOVELTY - Producing (M1) a chemoresistive organic vapor sensor, comprises e.g.: (a) mixing powder of at least 99.8% metallic niobium, at least 99% graphite and at least 95% aluminum carbide in a weight ratio of 2:1.2:1 in a laboratory drunk barrel type mixer for 24 hours until a homogeneous mixture is formed; (b) placing obtained mixture in a corundum crucible, transferring to a horizontal furnace, heating for purpose of sintering to 1580-1600° C at a rate of 5-10° C/minutes in an argon environment, holding for 8-10 hours, and cooling to room temperature; (c) removing sintered mixture (niobium aluminum carbide) from crucible, grinding resultant to obtain a powder consisting of particles less than 25 μ m in size; and (d) for the purpose of etching, adding 1 g nanolaminated niobium aluminum carbide powder to a Teflon(RTM: PTFE) reactor with solution containing 20 ml 9 M, at least 37% hydrochloric acid and 3.2 g, 99.9% lithium fluoride and continuously stirring using magnetic stirrer. USE - The methods are useful for producing chemoresistive organic vapor sensor and chemoresistive organic vapor sensor (claimed). ADVANTAGE - None given. DETAILED DESCRIPTION - Producing (M1) a chemoresistive organic vapor sensor, comprises: (a) mixing powder of at least 99.8% metallic niobium, at least 99% graphite and at least 95% aluminum carbide in a weight ratio of 2:1.2:1 in a laboratory drunk barrel type mixer for 24 hours until a homogeneous mixture is formed; (b) placing the obtained mixture in a corundum crucible, transferring to a horizontal furnace, heating for the purpose of sintering to 1580-1600° C at a rate of 5-10° C/minutes in an argon environment, holding for 8-10 hours, and cooling to room temperature; (c) removing the sintered mixture (niobium aluminum carbide) from the crucible, grinding resultant to obtain a powder consisting of particles less than 25 μ m in size; (d) for the purpose of etching, adding 1 g nanolaminated niobium aluminum carbide powder to a Teflon(RTM: PTFE) reactor with a solution containing 20 ml 9 M, at least 37% hydrochloric acid and 3.2 g, 99.9% lithium fluoride and continuously stirring using a magnetic stirrer for 90-96 hours at 50-55° C until the reaction between aluminum atoms and fluorides is complete and the bonds between niobium and aluminum atoms are broken, resulting in the formation of multilayer niobium carbide structures consisting of niobium aluminum carbide-Tx MXenes, where the surface of which is terminated by functional groups, mainly fluorine, oxygen and hydroxy ions; (e) subjecting obtained suspension to repeated washing from byproducts of the aluminum fluoride reactions in distilled water by centrifugation at a speed of 5500-6000 revolution per minute for 5-6 minutes until neutral pH values are 5-6; (f) filtering the stable black suspension and drying under reduced pressure i.e. below 103Pa for at least 24 hours at 80± 5° C to collect the exfoliated structures of two-dimensional MXenes;(g) placing obtained MXenes powder in distilled water to form a suspension in a ratio of 5-10 g/l and subjecting to ultrasonic treatment for 0.5-2 hours; (h) applying the suspension to a dielectric substrate equipped with strip measuring electrodes to form a layer of MXenes on its surface, or to a dielectric substrate not equipped with measuring electrodes, and later applying measuring electrodes over the MXene layer by cathode or magnetron sputtering using shadow masks and other microelectronic manufacturing methods; (i) drying resultant at up to 60° C until the liquid phase is removed; (j) welding the substrate with the applied layer of MXenes into a holder containing two measuring electrodes; and (k) annealing at 300° C in air for at least 24 hours to form an oxide phase on the surface of the MXenes. INDEPENDENT CLAIMS are also included for: producing (M2) a chemoresistive multisensor chip, comprising the steps (a)-(e) as per se, filtering the stable black suspension and drying under reduced pressure i.e. below 10 Pa for at least 24 hours at 80± 5° C to collect the exfoliated structures of two-dimensional MXenes, the steps (g)-(i) as per se, welding the substrate with the applied layer of MXenes into a holder containing more than three electrical leads, and the step (k) as per se; chemoresistive sensor of organic vapors obtained by the method (M1), where a layer of oxidized two-dimensional MAxene is used as the gas-sensitive material, placed on a dielectric substrate between two measuring electrodes, and the resistance of which changes when heated to 300° C under the influence of organic vapors and humidity in the surrounding air; and chemoresistive-type multisensor chip obtained by the method (M2), where a layer of oxidized two-dimensional MAxene is used in its composition, the layer enclosed between each pair of electrodes forms a sensor, and the entire set of sensors forms a multisensor line.
IPC 分类号G01N-027/12
国家俄罗斯
专业领域化学化工
语种英语
成果类型专利
文献类型科技成果
条目标识符http://119.78.100.226:8889/handle/3KE4DYBR/21819
专题中国科学院新疆生态与地理研究所
作者单位
UNIV SARAT STATE TECH (UYSA-C)
推荐引用方式
GB/T 7714
PLUGIN I A,POZNIAK A I,VAREZHNIKOV A S,et al. Producing chemoresistive organic vapor sensor by e.g. mixing powder of metallic niobium, graphite and aluminum carbide, placing mixture in crucible, transferring, heating, cooling, removing mixture, grinding and adding powder to reactor. RU2023113251-A; EA48111-B1[P]. 2023.
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