RuO2/ZrO2/TaON复合光催化材料的制备及光解水制氢性能

doi:10.15541/jim20150091

摘要/Abstract

摘要：

采用控制水解法制备了细颗粒的ZrO₂/Ta₂O₅复合氧化物粉体, 在氨气流量为90 mL/min、850℃下氮化10 h获得ZrO₂/TaON, 用浸渍法制备含助催化剂RuO₂的复合光催化剂。用XRD、SEM、TEM和UV-Vis漫反射光谱等对所制备的光催化材料进行了表征, ZrO₂、RuO₂的晶粒尺寸约为10 nm,TaON的晶粒尺寸约为25 nm, 复合光催化剂可以吸收波长≤500 nm的可见光。ZrO₂的引入降低了氮化生成TaON的缺陷密度, 提高了TaON的比表面积。光电流及光催化分解水制氢反应定量评价了复合材料的光催化性能, RuO₂含量为2.0wt%时复合光催化剂活性最高, 0.6 V偏压下光电流密度为0.6 mA/cm², 产氢速率为6.0 μmol/h。

关键词: 分解水, 析氢, 光催化, RuO2/ZrO2/TaON, 可见光

Abstract:

ZrO₂/Ta₂O₅ composite oxide powders in a fine particle size were prepared by the controlled hydrolysis method, and subsequently nitrided in a flowing ammonia at a flow rate of 90 mL/min at 850℃ for 10 h, to form ZrO₂/TaON. Then, RuO₂ co-catalyst was immobilized on the ZrO₂/TaON via an impregnation method. The samples were characterized with XRD, SEM, TEM and UV-Vis diffuse reflectance spectroscope. Both ZrO₂ and RuO₂ were in a crystallite size of ca. 10 nm, while TaON was in a crystallite size of ca. 25 nm, and composite photocatalysts absorbed the visible light at wavelength less than 500 nm. The introducing of ZrO₂ reduced the defect density of TaON and increased the specific surface area of TaON. The photocatalytic efficiency of composite photocatalysts was quantitatively evaluated via determining the photo-current density as well as in the water splitting hydrogen evolution reaction. The sample with a RuO₂ loading of 2.0wt% showed the photocurrent of 0.6 mA/cm² at a bias voltage of 0.6 V, and H₂ evolution rate as high as 6.0 μmol/h under a Xe lamp irradiation.

Key words: water splitting, hydrogen evolution, photocatalysis, RuO2/ZrO2/TaON, visible light

中图分类号:

TB321

郭冬雪, 张青红, 王宏志, 李耀刚, 曹广秀. RuO₂/ZrO₂/TaON复合光催化材料的制备及光解水制氢性能[J]. 无机材料学报, 2015, 30(10): 1025-1030.

GUO Dong-Xue, ZHANG Qing-Hong, WANG Hong-Zhi, LI Yao-Gang, CAO Guang-Xiu. Preparation of RuO₂/ZrO₂/TaON Composite Photocatalyst and Its Photocatalytic Properties for Water Splitting Hydrogen Evolution[J]. Journal of Inorganic Materials, 2015, 30(10): 1025-1030.

图/表 7

图1 850℃氨气流量为90 mL/min氮化10 h得到的ZrO2/TaON的XRD图谱

Fig. 1 XRD pattern of ZrO2/TaON nitrided at 850℃ for 10 h in a flowing NH3 of 90 mL/min

图2 TaON及ZrO2/ TaON的紫外-可见光漫反射光谱

Fig. 2 UV-Vis diffuse reflectance spectra of TaON and ZrO2/ TaON

图3 Ta2O5(a)、ZrO2/TaON(b)和b图局部放大(c)的场发射扫描电镜照片

Fig. 3 FE-SEM images of Ta2O5 (a), ZrO2/TaON (b) and enlarged image (c) of rectangle area in (b)

图4 ZrO2/TaON的透射电镜和高分辨透射电镜照片

Fig. 4 TEM (a) and HRTEM (b) images of ZrO2/TaON

图5 不同RuO2负载量RuO2/ZrO2/TaON的透射电镜及高分辨透射电镜照片

Fig. 5 TEM and HRTEM images of RuO2/ZrO2/TaON with different RuO2 loadings (a) 1.0wt%; (b) 1.0wt%; (c) 2.0wt%; (d) 3.0wt%

图6 可见光照射下ZrO2/TaON (a), 含不同RuO2的ZrO2/TaON光电流密度图

Fig. 6 Photocurrent densities under visible light irradiation of ZrO2/TaON (a) and RuO2/ZrO2/TaON photoanodes with different RuO2 loadings, 1.0wt% (b), 2.0wt% (c) and 3.0wt%(d)

图7 ZrO2/TaON (a), 含RuO21.0wt% (b), 2.0wt% (c), 3.0wt% (d)的ZrO2/TaON, 和含3.0wt%的RuO2的ZrO2/TaON(e)光催化分解水产氧速率-时间图

Fig. 7 Hydrogen production rates over photocatalysts ZrO2/ TaON (a) and RuO2/ZrO2/TaON with RuO2 loadings of 1.0wt% (b), 2.0wt% (c), 3.0wt% (d), and oxygen production rates over photocatalyst ZrO2/TaON with RuO2 loading of 3.0wt% (e)

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RuO₂/ZrO₂/TaON复合光催化材料的制备及光解水制氢性能

Preparation of RuO₂/ZrO₂/TaON Composite Photocatalyst and Its Photocatalytic Properties for Water Splitting Hydrogen Evolution

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