C-C模板的纳米二氧化钼制备研究
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摘要
以过氧钼酸为前驱体,腰果酚型酚醛树脂为模板,通过水热法制备了腰果酚型酚醛树脂/纳米氧化钼复合材料,最后再进行高温加热处理,制备得到C-C模板的纳米二氧化钼,并采用FT-IR、XRD、TEM和SEM等仪器对Mo O2高温处理前后的表面形貌进行了观测分析,同时采用XPS对材料表面元素组成进行分析。结果表明:在550℃处理3 h后的纳米二氧化钼呈粉末状,淡黄色。XPS检测显示纳米二氧化钼表面存在C、Mo、O等元素,且这些元素均以不同结合态存在,如Mo-C,O-C-O等。TEM检测显示有明显的C-C纤维模板,而SEM照片中可以清晰的观测到纳米二氧化钼以透明的棒状结构存在,高温处理使其晶型结构更为规整。
Using peroxo-polymolybdic acid as precursor,phenolic resin based on cardanol as template,nano-molybdenum oxide/phenolic resin based on cardanol composite was prepared via hydrothermal method,which was experienced with thermal treatment under 350 ℃ and 550 ℃ for 3 hours,respectively.Nano-MoO_2 with C-C template was obtained finally.The morphological and performance of the product were characterized by FT-IR、XRD、TEM and SEM.The surface composition of nano-MoO_2 was analyzed by XPS. All the data demonstrated that nano-MoO_2 obtained treated under 550 ℃ for 3 hours was a kind of powder with paint yellow,and C,Mo and O existed on its surface,the binding energy showed all these elements existed with different states,such as Mo-C,O-C-O,which was confirmed by XPS.C-C template were observed among TEM images,and SEM images showed there was flake sheet of transparent crystal structure,which structure tend to more neat under higher thermal treatment.
Using peroxo-polymolybdic acid as precursor,phenolic resin based on cardanol as template,nano-molybdenum oxide/phenolic resin based on cardanol composite was prepared via hydrothermal method,which was experienced with thermal treatment under 350 ℃ and 550 ℃ for 3 hours,respectively.Nano-MoO_2 with C-C template was obtained finally.The morphological and performance of the product were characterized by FT-IR、XRD、TEM and SEM.The surface composition of nano-MoO_2 was analyzed by XPS. All the data demonstrated that nano-MoO_2 obtained treated under 550 ℃ for 3 hours was a kind of powder with paint yellow,and C,Mo and O existed on its surface,the binding energy showed all these elements existed with different states,such as Mo-C,O-C-O,which was confirmed by XPS.C-C template were observed among TEM images,and SEM images showed there was flake sheet of transparent crystal structure,which structure tend to more neat under higher thermal treatment.
引文
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[3]Chen S,Qin X.Molybdenum oxide-iron oxide/graphene composite as anode materials for lithium ion batteries[J].Journal of Solid State Electrochemistry,2015,19(6):1867-1874.
[4]Xue X,Zhou Z,Peng B,et al.Review on nanomaterials synthesized by vapor transport method:growth and their related applications[J].RSC Advances,2015,5:79249-79263.
[5]Il’in E G,Beirakhov A G,Yarzhemskii V G,et al.Symmetric cage structures of isomers of nonstoichiometric lower molybdenum oxides[J].Doklady Chemistry,2017,475(2):173-178.
[6]Tian M,Chen L,Sekine H,et al.Crystal growth and physical properties of ternary bismuth molybdenum oxides Bix Mo Oy(x=0.21,0.25;y=3+δ)[J].Journal of Materials Science:Materials in Electronics,1998,9(1):25-29.
[7]石晓波,石淑华,李苑,等.纳米钼钒砷杂多酸盐催化苯羟化合成苯酚的研究[J].化学研究与应用,2005,17(6):783-785.
[8]Naoaki K,Nobuko K,Kazuo T.Electrochemical characteristics and structural changes of molybdenum trioxide hydrates as cathode materials for lithium batteries[J].Journal of Applied Electrochemistry,1988,18(6):857-862.
[9]石晓波,李春根,汪德先,等.过渡金属钼钒砷酸盐纳米微粒的固相合成与表征[J].化学研究与应用,2004,16(5):619-622.
[10]刘颖,冯金朝,李静.模板法制备α-o O3纳米棒和纳米矩形片及光谱表征[J].光谱学与光谱分析,2012,32(2):496-500.
[11]Zohreh R R,Iran S.Ultrasonic assisted preparation of nano-plate molybdenum(VI)coordination complex as a precursor for molybdenum trioxide nanoparticles preparation[J].Res Chem Intermed,2015,41:955-963.
[12]Cordier S,Grasset F,Molard Y,et al.Inorganic molybdenum octahedral nanosized cluster units,versatile functional building block for nanoarchitectonics[J].J Inorg Organomet Polym,2015,25:189-204.
[13]Sugumaran S J,Rathinam Y,Rangaraj S P,et al.Facile and novel synthetic method to prepare nano molybdenum and its catalytic activity[J].IET Nanobiotechnology,2015,9(4):201-208.
[14]Cristian F,Silvia C C,Pedro D V,et al.Highly selective and recyclable Mo O3nanoparticles in epoxidation catalysis[J].Applied Catalysis A:General,2015,504:344-350.
[15]Chu F,Li C,Wang Z,et al.Aluminum nitride thin films on molybdenum/polyimide heterostructure for bulk acoustic resonators[J].Rare Metal Materials and Engineering,2013,42(10):2023-2026.
[16]Ayeong B,Hatter C B,Jae H P,et al.Molybdenum oxide/carbon composites derived from the CO2oxidation of Mo2CTx(MXene)for lithium ion battery anodes[J].Electrochimica Acta,2017,258:979-987.
[17]Jin K K,Jong H K,Yun C K.Electrochemical properties of multicomponent oxide and selenide microspheres containing Co and Mo components with several tens of vacant nanorooms synthesized by spray pyrolysis[J].Chemical Engineering Journal,2018,333:665–677.