本實驗以硝酸鉍、鈦異丙醇、檸檬酸為起始原料，進行溶膠-凝膠法成功合成可見光驅動之水分解氧化觸媒 Bi20TiO32。溶膠-凝膠法的初始為非晶相，在375oC空氣環境下進行煅燒6小時，並藉由Ｘ-ray 光繞射分析、 穿透式電子顯微鏡以及可見光-近紅外光漫反射光譜，進行晶格結構、 晶粒大小以及光吸收特性之鑑定。於溶膠-凝膠法時，檸檬酸與金屬離子之比例增加時會導致Bi20TiO32之晶粒增大，因而降低其氧氣生成之效率。
本觸媒的催化活性分別在紫外線與可見光光譜下進行活性測定。在實驗中以硝酸銀作為犧牲劑，並在研究中深入探討了犧牲劑濃度與鉑/銥氧化物共觸媒的添加對於其光催化活性之影響。犧牲劑之濃度與氧氣生成量為一線性成長之關係，當銥氧化物含量為0.15 wt%及鉑含量為0.2wt%時可以分別得到最大之氧氣生成量為6.47 mol/min及5.8 mol/min。而當共觸媒於鉑含量0.1 wt%及銥氧化物含量0.11 wt%時，則可以得到最佳之氧氣生成量為7 mol/min。
此外，在水分解的測試上，以產氧觸媒Bi20TiO32與產氫觸媒CuFeO2，以光沉積法還原石墨烯且添加共觸媒Ru/IrO2進行整合，成功將其導入單槽與雙槽之Z-scheme水分解架構。 於光觸媒含量Bi20TiO32 – CuFeO2分別為 0.1 – 0.1，0.05 – 0.05 及0.03 – 0.03克時，並無任何氣體生成。但分別加入3 wt%之還原石墨烯於兩光觸媒時則可大幅提升其光觸媒活性，於Bi20TiO32 – CuFeO2光觸媒含量為0.015 – 0.015克時可於12小時UV光照射下，生成氣體13.4 mol。最後，以3 wt% 還原石墨烯及共觸媒0.15 wt%銥氧化物及0.2 wt%銣之使用可增進光觸媒之水分解效率，其氫氣產量為2.23 mol/hour，氧氣為1.15 mol/hour。初步結果顯示此系統未來於水分解上之應用潛力。

Solar light driven water oxidation photocatalyst Bi20TiO32 has been successfully synthesized through sol gel process using bismuth nitrate, titanium isopropoxide and citric acid as starting materials. The amorphous metal oxides resulted from sol gel process was calcined at 375oC for 6 hour under stagnant air. Crystal structure and domain size of Bi20TiO32 were characterized by XRD and TEM. Optical properties of Bi20TiO32 were determined by UV-Visible spectroscopy as well. The increasing of citric acid ratio to the total metal ions increases the grain size of Bi20TiO32 due to more stable complex occurred in sol-gel process which finally decreases the photocatalytic activity oxygen evolution due to decreasing of total surface area.
Photocatalytic activity for oxygen evolution using silver nitrate as sacrificial agent under UV light and visible light irradiation have also been studied and enhanced by the addition of co-catalyst iridium oxide and platinum to the photocatalyst. The effects of sacrificial agent concentration, iridium oxide and platinum loading have been studied extensively. Increasing sacrificial agent concentration increases the initial rate of oxygen evolution with a linear relationship. Iridium oxide co-catalyst loading only gives maximum initial rate at 0.15 wt% loading while platinum only at 0.2 wt% with initial gas evolution rate 6.47 mol/min and 5.8 mol/min respectively. Loading iridium oxide and platinum co-catalyst simultaneously further increases the initial rate of oxygen evolution to 7 mol/min for 0.11 wt% iridium oxide with 0.1 wt% platinum.
Furthermore, overall water splitting reaction using Bi20TiO32 in combination with CuFeO2 has also been conducted by Z-scheme process in both single and twin reactor. Single reactor Z-scheme process conducted using only photocatalyst gives no gas evolution for various loading of Bi20TiO32 – CuFeO2 photocatalyst as 0.1 – 0.1, 0.05 – 0.05 and 0.03 – 0.03 gram. Addition of 3 wt% photo-reduced graphene oxide to both photocatalyst can enhance the photocatalytic activity as indicated by evolution of 13.4 mol gas for 12 hour UV illumination using 0.015 –0.015 gram Bi20TiO32 – CuFeO¬2 photocatalyst. Finally, 3 wt% of photo-reduced graphene oxide and co-catalyst 0.15 wt% iridium oxide and 0.2 wt% ruthenium have been used to further enhance photocatalytic activity water splitting resulting on the evolution of 2.23 mol/hour hydrogen and 1.15 mol/hour oxygen. All these initial results reveal that the potential on the application of water splitting.

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