| Ti基表面NiO修饰纳米TiO2电极材料的制备及电催化活性 |
| Electro-catalytic Activity and Preparation of Nano-crystalline TiO2/Ti Electrode Material Modified by NiO |
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| 摘要: 在无水乙醇和乙酰丙酮混合溶液中，电解Ti、Ni金属制得电极材料前驱体NiTim(OR)3m+1(acac)m+1。将其直接水解、干燥后在550 ℃煅烧2 h，制得纳米NiO/TiO2粉体。通过红外光谱(FTIR)、X射线衍射(XRD)、电子透射显微镜(TEM)测试表明，前驱体中含有乙酰丙酮基[acac-]，颗粒平均尺寸为20 nm。通过电合成与沉积得到高活性的纳米NiO/TiO2修饰电极，采用循环伏安和循环方波伏安研究NiO/TiO2电极在H2SO4溶液中的氧化还原行为以及还原草酸的电催化活性。结果表明，NiO/TiO2电极在1 mol·L-1
H2SO4溶液中有两对氧化还原峰Epc1=-0.61 V，Epc2=-1.05 V(vs
SCE)，掺杂Ni电极的放电电流明显增大，达75 mA·cm-2。间接电还原草酸为乙醛酸，收率和电流效率分别达93%和96%。 |
| 关键词: 金属醇盐 纳米TiO2电极 NiO 电催化 草酸 |
| 基金项目: |
| Abstract: The precursor NiTim(OR)3m+1(acac)m+1 was synthesized by electrolysis of titanium and nickel in absolute ethanol and acetyl-acetone solution. Nano-crystalline
NiO/TiO2 powder was prepared by direct sol-gel method from the precursor and then calcined for 2 h at 550 ℃. FTIR, XRD and TEM results showed that the precursor containing
acac- group and nano-NiO/TiO2 of 20 nm was obtained. The highly active
nano-NiO/TiO2 modified electrode was prepared using electro-synthesis and electro-deposition. The cyclic voltammetry and osteryoung square wave were used to study the redox behavior of the
nano-NiO/TiO2 electrode in H2SO4 solution. There were two pairs of well-defined redox peaks for the
nano-NiO/TiO2 electrode in 1 mol·L-1 H2SO4 with
Epc1=-0.61 V，Epc2=-1.05 V (vs SCE) at 100 mV·s-1. The discharge current of
nano-Ni/TiO2 electrode increased obviously and current density reached to 75 mA·cm-2. The heterogeneous electro-catalytic activities of this electrode in oxalic acid was investigated. In preparative electrolysis under optimal conditions, the average yield and current efficiency for glyoxalic acid were 93% and 96% respectively. |
| Keywords: metal alkoxide nano-meter TiO2 NiO electro-catalysis oxalic acid |
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| 朱传高,褚道葆.Ti基表面NiO修饰纳米TiO2电极材料的制备及电催化活性[J].无机化学学报,2006,22(2):223-227. |
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