摘要
采用阳极氧化法在Fe上原位生长直立有序的Fe2O3纳米管阵列,脉冲电沉积法将蜂窝状CuO组装到Fe2O3NTs上,得到CuO HCs/Fe2O3NTs催化剂.结果表明:Fe2O3NTs呈"火山状"规则生长,蜂窝状CuO均匀分布在Fe2O3NTs表面.修饰后,材料的能隙由原来的2.03 eV窄化为1.84 eV.同时发现该催化剂具有优良的光催化还原性能和电催化还原性能,光电催化还原CO2的主要生成产物为甲醇,甲醇在6 h时含量峰值为3.77 mmol/L.该研究对光电催化还原CO2有一定的指导和借鉴意义.
Vertically aligned Fe2O3 nanotubes （Fe2O3 NTs） arrays were prepared on the iron foil by potentiostatic anodization method. The anodization experiments were performed under 30 V for 2 h （20 ℃）. The ferrous foil was working electrode and titanium foil was counter electrode. The electrolytes were consisted of 0.25 wt% NH4F in an aqueous solution （Volume of water：glycol=3：97）. After sonicating for 5 min, the samples were put under oxygen atmosphere with the flow rate of 60 sccm （standard cubic centimeters/min） and heated to 500 ℃ with the rate of 3 ℃？min-1 and maintained at 500 ℃ for 2 h. Then cooled to room temperature with the rate of 3 ℃？min-1. Honeycomb structure cupric oxide （CuO HCs） were decorated on the surface of Fe2O3 NTs by the pulse electrochemical deposition method. This was done by CHI660D potentiostat in 1 mol？L-1 CuSO4 solution （40 ℃） in a three-electrode configuration. The Fe2O3 NTs electrode worked as counter electrode, Hg/Hg2Cl2 in saturated KCl solution as reference electrode, and platinum wire as working electrode, respectively. A 10 ms cathodic pulse with a current density of -70 mA？cm-2 was employed. After that followed by a 1 ms anodic pulse and its density was ＋70 mA？cm-2 to prevent damage of the Fe2O3 NTs structure. Finally was a 1000 ms rest time. The electrodeposition time was 36 s, with a forward duty cycle of 0.99% （considering cathodic, anodic and rest components）. Then the samples were annealed under oxygen atmosphere with the flow rate of 60 sccm then heated to 300 ℃ with the rate of 3 ℃？min-1 and maintained at 300 ℃ for 2 h. Then cooled to room temperature with the rate of 3 ℃？min-1. Then the CuO HCs/Fe2O3 NTs catalysis was obtained. The SEM images showed that CuO HCs distributed uniformly on the surface of Fe2O3 NTs that arranged in order were volcano-like. Measured by UV-vis DRS （ultraviolet-visible diffuse reflection spectrum） and valence band photoemission spectrum, its band energy has been narrowed from 2.03
出处
《化学学报》
SCIE
CAS
CSCD
北大核心
2013年第6期941-946,共6页
Acta Chimica Sinica
基金
国家青年自然科学基金(No.21203114)
山东省优秀中青年科学家科研奖励基金(No.BS2012NJ008)
山东京博控股股份有限公司资助~~
