TiO_2及TiO_2-碳质材料复合物的制备及其催化性能的研究
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摘要
由于高比表面积、优良的光致催化活性以及良好的生物兼容性,TiO2纳米材料在酶固载、光催化和光伏领域中受到极大的关注。然而,目前对于具有高电化学活性的特殊纳米结构TiO2薄膜及其酶固载几乎没有报道。另外,当TiO2纳米材料作为光催化剂使用时,其光催化效率较低,并且纳米TiO2粉体也难以回收。针对这些问题,我们采用液相沉积法分别制备了SDS掺杂的TiO2薄膜、CNTs-TiO2复合薄膜及氧化石墨烯-TiO2复合物,并研究其电催化和光催化性能。
以表面活性剂十二烷基磺酸钠(SDS)同时作为掺杂剂和结构诱导剂,以(NH4)2TiF6为TiO2前躯体,采用液相沉积方法,在室温下制备SDS掺杂的TiO2薄膜。SEM分析表明：该薄膜由底层的TiO2纳米颗粒层和上层的TiO2纳米片层组成,上层的TiO2纳米片垂直于基底表面,且自组装成花状结构。SDS的浓度对TiO2形状的转换起到了关键作用。低浓度SDS时,基底表面只有TiO2颗粒产生；高浓度的SDS有利于TiO2纳米片的形成。制备TiO2纳米片的最佳温度为308℃。SDS掺杂后,TiO2的循环伏安图中羟基化的Ti(Ⅳ)的还原峰明显增强。此外,SDS-TiO2薄膜可以作为良好的载体用于固定血红蛋白(Hb),并且该电极对H2O2有良好的电催化还原活性。作为分析H2O2的电化学传感器,固定Hb的薄膜电极对0.003至1.5 mM范围内的H2O2具有良好的线性关系,检出限为1.0μM。
采用浸渍-提拉和液相沉积两步法制备了碳纳米管(CNTs)和TiO2的复合物薄膜,并通过甲基橙的降解研究了复合薄膜的光电催化性质。结果表明,CNTs能够显著减小TiO2薄膜的电荷转移电阻,提高薄膜在紫外光照时的光电流响应。CNTs-TiO2复合薄膜的光电催化性能可以通控制制备时的沉积时间、煅烧温度等参数调节。沉积时间和煅烧温度分别为1 h和450℃,复合薄膜的光电催化活性最高。此时,复合薄膜在90 min内可将10 mg/L甲基橙降解95%,远高于单纯TiO2薄膜60%的降解率。
基于液相沉积法提出了一种在氧化石墨烯表面原位沉积TiO2纳米粒子制备高效光催化剂的简单方法。本方法的最主要的优点在于：纳米TiO2颗粒在氧化石墨烯片表面组装得到微米尺寸的光催化剂,该催化剂可以通过简单过滤而分离。SEM和BET等表征表明：二维多孔结构的氧化石墨烯-Ti02复合物比表面积为80 m2/g,明显高于P25和相同方法制备的Ti02。氧化石墨烯-Ti02极高的光催化受煅烧温度、氧化石墨烯含量以及溶液pH的影响。在最优条件下(氧化石墨加入浓度为75 mg／L,200℃煅烧),复合物光催化氧化甲基橙和光催化还原的Cr(Ⅵ)的速率分别是P25的7.4倍和5.4倍。氧化石墨烯能显著增强Ti02光催化活性是因为复合物中热处理后的氧化石墨烯独特的二维片状结构、大的比表面积和增强的吸附能力、以及强的电荷转移能力。
TiO2 nanomaterials have attracted particular attention due to its fascinating properties, such as high surface area, photoinduced activities and good biocompatibility for their uses in the fields such as in enzyme immobilization, photocatalysis and photovoltaics. Nevertheless, few papers involved the improved electrochemical activity of TiO2 film with special nanostructure and the immobilization of enzyme on it have been reported. On the other hand, when TiO2 nanomaterial was used as a photocatalyst, its photocatalyic efficiency is usually very low and easily subjected to the loss of TiO2 nanomaterial and the difficulty in the recovery of TiO2.Based on these problems, we have prepared SDS-doped TiO2 film、CNTs-TiO2 and graphene oxide-TiO2 composite with the liquid phase deposition and applied these composite in the field of electrocatalysis and phtotocatalysis.
With the surfactant sodium dodecyl sulfonate (SDS) as a dopant and structure director and (NH4)2TiF6 as the TiO2precursor, SDS-doped TiO2 film has been fabricated at room temperature. The SEM characterization showed that the TiO2 film was composed of two layers:the bottom layer with TiO2 grains and the top layer consisted of nanosheets, which are aggregated to a flower-like shape. The SDS concentration played a key role on the shape evolution of TiO2:a lower SDS concentration resulted in the formation of only TiO2 grains, and a higher SDS concentration was favorable to the growth of TiO2 nanosheets. And the optimum temperature was found to be 30 (?) for the growth of TiO2 nanosheets. After being doped with SDS, the reduction peak, being attributed to the reduction of hydroxylated titanium(Ⅳ) species, in the cyclic voltammograms of TiO2 films was siglifictantly enhanced. The varied surface structure of the SDS-doped TiO2 film provided a biocompatible platform for immobilizing hemoglobin, and the hemoglobin-immobilized film electrode exhibited good electrocatalytic activity to the reduction of H2O2. As a sensor for the determination of H2O2, the hemoglobin-immobilized film electrode yielded an excellently linear range from 0.003 to 1.5 mM H2O2 in the correlation between reduction peak current and H2O2 concentration, with a low detection limit of 1.0μM.
Composite films of TiO2 and carbon nanotubes (CNTs) were prepared on titanium sheets with a dip-coating and liquid phased deposition and the photoelectrocatalytic (PEC) properties of the films were investigated through the degradation of methyl orange. It was demonstrated that CNTs in the TiO2 film significantly decreased the charge transfer resistance and increased the anodic photocurrent response of the film under UV light irradiation. The PEC performance of the CNTs-based composite film could be tuned by controlling the preparation parameters including the deposition time and calcination temperature. The deposition time and calcination temperature were optimized at 1 h and 450 (?), respectively. On the TiO2/CNT film prepared under the optimized conditions, 95% of the initial 10 mg/L methyl orange was degraded within 90 min, which was much higher than the 60% removal seen on the pure TiO2 films.
Based on liquid phased depositon, a simple method to synthesize graphene oxide/TiO2 composites as a highly efficient photocatalyst by in situ depositing TiO2 nanoparticles on graphene oxide nano-sheets was developed. There are several advantages for this method. TiO2 nanoparticles are assembled onto the graphene oxide sheet to form larger particle s in the microscale, which could be easily separated by the filtration. Additionally, SEM and BET characterization showed the two-dimensional porous graphene oxide/TiO2 composites had specific surface area of 80 m2 g"1 being considerably larger than that of P25 and the similarly prepared neat TiO2 particles without using graphene oxide. The composites exhibited excellent photocatalytic activity, being influenced by post-calcination temperature, graphene oxide content and solution pH. Under optimal conditions (the concentration of graphite oxide was 75 mg/mL and calcination temperature was 200 (?)), the photo-oxidative degradation rate of methyl orange and the photo-reductive conversion rate of Cr(Ⅵ) over the composites were as high as 7.4 and 5.4 times that over P25, respectively. The excellent enhancing effect of graphene oxide nano-sheets on the photocatalytic properties of TiO2 was attributed to a thin two-dimensional sheet support, a large surface area and much increased adsorption capacity, and the strong electron transfer ability of the thermally treated graphene oxide in the composite.
以表面活性剂十二烷基磺酸钠(SDS)同时作为掺杂剂和结构诱导剂,以(NH4)2TiF6为TiO2前躯体,采用液相沉积方法,在室温下制备SDS掺杂的TiO2薄膜。SEM分析表明：该薄膜由底层的TiO2纳米颗粒层和上层的TiO2纳米片层组成,上层的TiO2纳米片垂直于基底表面,且自组装成花状结构。SDS的浓度对TiO2形状的转换起到了关键作用。低浓度SDS时,基底表面只有TiO2颗粒产生；高浓度的SDS有利于TiO2纳米片的形成。制备TiO2纳米片的最佳温度为308℃。SDS掺杂后,TiO2的循环伏安图中羟基化的Ti(Ⅳ)的还原峰明显增强。此外,SDS-TiO2薄膜可以作为良好的载体用于固定血红蛋白(Hb),并且该电极对H2O2有良好的电催化还原活性。作为分析H2O2的电化学传感器,固定Hb的薄膜电极对0.003至1.5 mM范围内的H2O2具有良好的线性关系,检出限为1.0μM。
采用浸渍-提拉和液相沉积两步法制备了碳纳米管(CNTs)和TiO2的复合物薄膜,并通过甲基橙的降解研究了复合薄膜的光电催化性质。结果表明,CNTs能够显著减小TiO2薄膜的电荷转移电阻,提高薄膜在紫外光照时的光电流响应。CNTs-TiO2复合薄膜的光电催化性能可以通控制制备时的沉积时间、煅烧温度等参数调节。沉积时间和煅烧温度分别为1 h和450℃,复合薄膜的光电催化活性最高。此时,复合薄膜在90 min内可将10 mg/L甲基橙降解95%,远高于单纯TiO2薄膜60%的降解率。
基于液相沉积法提出了一种在氧化石墨烯表面原位沉积TiO2纳米粒子制备高效光催化剂的简单方法。本方法的最主要的优点在于：纳米TiO2颗粒在氧化石墨烯片表面组装得到微米尺寸的光催化剂,该催化剂可以通过简单过滤而分离。SEM和BET等表征表明：二维多孔结构的氧化石墨烯-Ti02复合物比表面积为80 m2/g,明显高于P25和相同方法制备的Ti02。氧化石墨烯-Ti02极高的光催化受煅烧温度、氧化石墨烯含量以及溶液pH的影响。在最优条件下(氧化石墨加入浓度为75 mg／L,200℃煅烧),复合物光催化氧化甲基橙和光催化还原的Cr(Ⅵ)的速率分别是P25的7.4倍和5.4倍。氧化石墨烯能显著增强Ti02光催化活性是因为复合物中热处理后的氧化石墨烯独特的二维片状结构、大的比表面积和增强的吸附能力、以及强的电荷转移能力。
TiO2 nanomaterials have attracted particular attention due to its fascinating properties, such as high surface area, photoinduced activities and good biocompatibility for their uses in the fields such as in enzyme immobilization, photocatalysis and photovoltaics. Nevertheless, few papers involved the improved electrochemical activity of TiO2 film with special nanostructure and the immobilization of enzyme on it have been reported. On the other hand, when TiO2 nanomaterial was used as a photocatalyst, its photocatalyic efficiency is usually very low and easily subjected to the loss of TiO2 nanomaterial and the difficulty in the recovery of TiO2.Based on these problems, we have prepared SDS-doped TiO2 film、CNTs-TiO2 and graphene oxide-TiO2 composite with the liquid phase deposition and applied these composite in the field of electrocatalysis and phtotocatalysis.
With the surfactant sodium dodecyl sulfonate (SDS) as a dopant and structure director and (NH4)2TiF6 as the TiO2precursor, SDS-doped TiO2 film has been fabricated at room temperature. The SEM characterization showed that the TiO2 film was composed of two layers:the bottom layer with TiO2 grains and the top layer consisted of nanosheets, which are aggregated to a flower-like shape. The SDS concentration played a key role on the shape evolution of TiO2:a lower SDS concentration resulted in the formation of only TiO2 grains, and a higher SDS concentration was favorable to the growth of TiO2 nanosheets. And the optimum temperature was found to be 30 (?) for the growth of TiO2 nanosheets. After being doped with SDS, the reduction peak, being attributed to the reduction of hydroxylated titanium(Ⅳ) species, in the cyclic voltammograms of TiO2 films was siglifictantly enhanced. The varied surface structure of the SDS-doped TiO2 film provided a biocompatible platform for immobilizing hemoglobin, and the hemoglobin-immobilized film electrode exhibited good electrocatalytic activity to the reduction of H2O2. As a sensor for the determination of H2O2, the hemoglobin-immobilized film electrode yielded an excellently linear range from 0.003 to 1.5 mM H2O2 in the correlation between reduction peak current and H2O2 concentration, with a low detection limit of 1.0μM.
Composite films of TiO2 and carbon nanotubes (CNTs) were prepared on titanium sheets with a dip-coating and liquid phased deposition and the photoelectrocatalytic (PEC) properties of the films were investigated through the degradation of methyl orange. It was demonstrated that CNTs in the TiO2 film significantly decreased the charge transfer resistance and increased the anodic photocurrent response of the film under UV light irradiation. The PEC performance of the CNTs-based composite film could be tuned by controlling the preparation parameters including the deposition time and calcination temperature. The deposition time and calcination temperature were optimized at 1 h and 450 (?), respectively. On the TiO2/CNT film prepared under the optimized conditions, 95% of the initial 10 mg/L methyl orange was degraded within 90 min, which was much higher than the 60% removal seen on the pure TiO2 films.
Based on liquid phased depositon, a simple method to synthesize graphene oxide/TiO2 composites as a highly efficient photocatalyst by in situ depositing TiO2 nanoparticles on graphene oxide nano-sheets was developed. There are several advantages for this method. TiO2 nanoparticles are assembled onto the graphene oxide sheet to form larger particle s in the microscale, which could be easily separated by the filtration. Additionally, SEM and BET characterization showed the two-dimensional porous graphene oxide/TiO2 composites had specific surface area of 80 m2 g"1 being considerably larger than that of P25 and the similarly prepared neat TiO2 particles without using graphene oxide. The composites exhibited excellent photocatalytic activity, being influenced by post-calcination temperature, graphene oxide content and solution pH. Under optimal conditions (the concentration of graphite oxide was 75 mg/mL and calcination temperature was 200 (?)), the photo-oxidative degradation rate of methyl orange and the photo-reductive conversion rate of Cr(Ⅵ) over the composites were as high as 7.4 and 5.4 times that over P25, respectively. The excellent enhancing effect of graphene oxide nano-sheets on the photocatalytic properties of TiO2 was attributed to a thin two-dimensional sheet support, a large surface area and much increased adsorption capacity, and the strong electron transfer ability of the thermally treated graphene oxide in the composite.
引文
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