• 专利标题:   Preparing tin disulfide/graphene/tin dioxide ternary composite gas sensing material for nitrogen dioxide sensor, involves preparing tin sulfide nanosheet under inert protection of atmosphere by adding tin tetrachloride pentahydrate.
  • 专利号:   CN108181355-A
  • 发明人:   WANG Y, ZHENG C
  • 专利权人:   HARBIN INST TECHNOLOGY
  • 国际专利分类:   G01N027/12, C01G019/00, C01B032/184, C01B032/194, C01G019/02
  • 专利详细信息:   CN108181355-A 19 Jun 2018 G01N-027/12 201851 Pages: 19 Chinese
  • 申请详细信息:   CN108181355-A CN11488163 29 Dec 2017
  • 优先权号:   CN11488163

▎ 摘  要

NOVELTY - Preparing tin disulfide/graphene/tin dioxide ternary composite gas sensing material involves preparing tin sulfide nanosheet under inert protection of the atmosphere by adding tin tetrachloride pentahydrate, oleic acid and octadecene to the three-necked flask, in a mass ratio of 0.37g:1mL:2mL, stirring at 100 degrees C, performing deoxidation and dehydration for 1 hours, then increasing temperature to 280 degrees C at temperature increase rate of 6 degrees C/minute, adding 5 mL sulfur oleylamine solution, where concentration of sulfur in sulfur oleylamine solution is 0.2 millimoles/mL. The reaction is carried out at 280 degrees C for 30 minutes, and reaction mixture is centrifuged by adding ethanol and cyclohexane. The product is collected by centrifugation, dispersed in water, diluted with hydrochloric acid, pH is adjusted to 3-4, and ultrasonicated for 2 hour at 200 Watt to obtain tin sulfide nanosheet. The diethyl ether is added to the aqueous solution of tin sulfide for 30 minutes at 200 Watts. USE - Method for preparing tin disulfide/graphene/tin dioxide ternary composite gas sensing material for nitrogen dioxide sensor. ADVANTAGE - The method enables to prepare tin disulfide/graphene/tin dioxide ternary composite gas sensing material high-sensitivity which realizes nitrogen dioxide sensitive response under low temperature and low detection limit. DETAILED DESCRIPTION - Preparing tin disulfide/graphene/tin dioxide ternary composite gas sensing material involves preparing tin sulfide nanosheet under inert protection of the atmosphere by adding tin tetrachloride pentahydrate, oleic acid and octadecene to the three-necked flask, in a mass ratio of 0.37g:1mL:2mL, stirring at 100 degrees C, performing deoxidation and dehydration for 1 hours, then increasing temperature to 280 degrees C at temperature increase rate of 6 degrees C/minute, adding 5 mL sulfur oleylamine solution, where concentration of sulfur in sulfur oleylamine solution is 0.2 millimoles/mL. The reaction is carried out at 280 degrees C for 30 minutes, and reaction mixture is centrifuged by adding ethanol and cyclohexane. The product is collected by centrifugation, dispersed in water, diluted with hydrochloric acid, pH is adjusted to 3-4, and ultrasonicated for 2 hour at 200 Watt to obtain tin sulfide nanosheet. The diethyl ether is added to the aqueous solution of tin sulfide for 30 minutes at 200 Watts, poured out the upper layer of diethyl ether, followed by the addition of diethyl ether, and poured out the upper layer of diethyl ether after ultrasonication for 30 minutes under the condition of power of 200 Watts, followed by the addition of ether for 30 minutes at 200 Watts, the upper layer of diethyl ether is poured out, and the lower dispersion is extracted to obtain tin sulfide, dispersed for removing the oleic acid ligand, which is collected by centrifugation and mixed with ethanol to obtain ethanol solution tin sulfide. The graphene and tin oxide quantum wire are added an 1.4-5 mL aqueous solution of ethanol and 0.28-1 mL graphite oxide are added to the quartz microwave reaction tube, and the concentration of graphene oxide in the aqueous solution of graphite oxide is 1 mg/mL, and then tin is added, Salt is added, and mixture is stirred at room temperature for 30 minutes to completely dissolve the tin tetrachloride. 2.8-10 mL oleic acid and 0.35-1.25 mL oleylamine are added to the reaction tube, and the reaction tube is placed in a microwave reactor, stirred for 30 s, at 180 degrees C, and reacted for 1 hours, the product is washed for 3 times with volume ratio of 1:1 ethanol and cyclohexane mixed solution, finally collected by centrifugation, dispersed in ethanol to obtain graphene/tin oxide quantum wire ethanol solution. The tin sulfide/graphene/tin oxide composite sensing film is prepared by firstly apply the ethanol solution of graphene/tin oxide quantum wire to the ceramic piece with the gold finger electrode and the size of electrode is 10x 815 millimeter.