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Preparation and characterisation of nanostructural TiO2-Ga2O3 binary oxides with high surface area derived form particulate sol-gel route

机译:溶胶-凝胶法合成高表面积纳米TiO2-Ga2O3二元氧化物的制备与表征

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摘要

Nanostructured and nanoporous TiO2Ga2O3 films and powders with various Ti:Ga atomic ratios and high specific surface area (SSA) have been prepared by a new straightforward particulate sol-gel route. Titanium isopropoxide and gallium (III) nitrate hydrate were used as precursors and hydroxypropyl cellulose (HPC) was used as a polymeric fugitive agent (PFA) in order to increase the SSA. X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) revealed that powders contained both rhombohedral alpha-Ga2O3 and monoclinic beta-Ga2O3 phases, as well as anatase and rutile. It was observed that the Ga2O3 formed from the nitrate precursor retarded anatase-to-rutile transformation. Furthermore, transmission electron microscope (TEM) analysis also showed that Ga2O3 hindered the crystallisation and crystal growth of powders. SSA of powders, as measured by Brunauer-Emmett-Teller (BET) analysis, was enhanced by introducing Ga2O3. Ti:Ga = 50:50 (at%/at%) binary oxide annealed at 500 degrees C produced the smallest crystallite size (2 nm), the smallest grain size (18 nm), the highest SSA (327.8 m(2)/g) and the highest roughness. Ti:Ga = 25:75 (at%/at%) annealed at 800 degrees C showed the smallest crystallite size (2.4 nm) with 32 nm average grain size and 40.8 m(2)/g surface area. Ti:Ga = 75:25 (at%/at%) annealed at 800 degrees C had the highest SSA (57.4 m(2)/g) with 4.4 nm average crystallite size and 32 nm average grain size. One of the smallest crystallite size and one of the highest SSA reported in the literature is obtained, and they can be used in many applications in areas from optical electronics to gas sensors.
机译:已经通过一种新的直接的颗粒溶胶-凝胶法制备了具有各种Ti:Ga原子比和高比表面积(SSA)的纳米结构和纳米多孔TiO2Ga2O3薄膜和粉末。异丙醇钛和水合硝酸镓(III)被用作前体,而羟丙基纤维素(HPC)被用作聚合逃犯剂(PFA),以提高SSA。 X射线衍射(XRD)和傅立叶变换红外光谱(FTIR)显示,粉末既包含菱形α-Ga2O3相,又包含单斜晶β-Ga2O3相,以及锐钛矿和金红石相。观察到,由硝酸盐前体形成的Ga 2 O 3抑制了锐钛矿到金红石的转化。此外,透射电子显微镜(TEM)分析还表明,Ga 2 O 3阻碍了粉末的结晶和晶体生长。通过引入Ga2O3可以提高通过Brunauer-Emmett-Teller(BET)分析测得的粉末的SSA。 Ti:Ga = 50:50(at%/ at%)在500摄氏度下退火的二元氧化物产生最小的微晶尺寸(2 nm),最小的晶粒尺寸(18 nm),最高的SSA(327.8 m(2)/ g)和最高的粗糙度。在800摄氏度下退火的Ti:Ga = 25:75(at%/ at%)显示了最小的微晶尺寸(2.4 nm),平均晶粒尺寸为32 nm,表面积为40.8 m(2)/ g。在800摄氏度下退火的Ti:Ga = 75:25(at%/ at%)具有最高的SSA(57.4 m(2)/ g),平均晶粒尺寸为4.4 nm,平均晶粒尺寸为32 nm。获得了文献中报道的最小的微晶尺寸之一和最高的SSA之一,它们可用于从光学电子到气体传感器的许多应用。

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