微纳结构催化剂的设计合成及其在光催化反应中的应用
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摘要
模拟自然界光合作用，构建人工光催化系统实现对太阳能的利用，是解决目前人类所面临的能源危机和环境污染问题的根本途径。具有良好的光电响应特性的纳米半导体材料为这一目标的实现提供了可能。然而，目前在半导体纳米光催化研究领域存在诸多问题，如光谱吸收范围窄、光生电子空穴易复合、氧化还原能力难控、牺牲剂难以避免等，导致其发展缓慢，特别是在实际应用方面鲜有报道。近年来，由主体半导体材料和电子供受体（或兼具光吸收功能）组装的功能化微纳结构光催化材料，因具有良好的光催化性能，受到人们的重视。然而，目前对微纳结构材料中电子供受体的形态、空间位置及有效吸光性对其光催化活性的影响研究鲜有报道。
在本文中，我们基于表面电子供受体形态控制、电子供受体空间限域、稀土上转换发光等研究策略，通过功能化微纳结构光催化剂的构建，为上述问题的解决提供了新途径。
首先，为了研究表面电子供受体形态对半导体光催化性能的影响，我们构建了具有蛇莓形态的TiO_2-Cdot微纳结构光催化体系，提供了一种TiO_2表面电子供受体碳纳米点的可控合成策略，探讨了碳纳米点分布对TiO_2光催化活性的影响，提出了TiO_2@C核壳结构在光催化过程中可能存在“活塞式”光生电子转移模式。通过对光催化剂吸附性能、光吸收程度、光电响应性能等研究，揭示TiO_2表面碳纳米点的形态是影响微纳结构TiO_2-C组装材料光催化活性的关键因素。
另外，在上述研究二氧化钛和碳复合材料的过程中，我们以碳为还原性物种将TiO_2部分还原，合成出了具有多面体自组装形貌的灰黑色金红石型TiO_2。与普通白色金红石型TiO_2相比，由于Ti3+的存在，使该灰黑色TiO_2具有很强的可见光吸收能力及光电分离能力；在可见光下，其光催化性能显著高于白色金红石型TiO_2和锐钛型P25TiO_2。并且，我们通过二次煅烧钝化TiO_2表面还原态Ti3+，有效提高了灰黑色TiO_2的物理化学稳定性及光催化活性的稳定性。
为了研究表面电子供受体空间位置对半导体光催化性能的影响，我们以TiO_2纳米管为基体，将Pt纳米粒子作为电子受体限域在TiO_2纳米管内部，将兼具光吸收天线和电子供体功能的TCMnPc限域在TiO_2纳米管外部，构建了具有电子供受体空间限域结构的Pt@TiO_2-TCMnPc光催化体系，提供了一种层层组装法和模板法相结合的空间限域微纳结构材料的通用性合成方法。在该微纳结构光催化体系中，电子供、受体作为反应活性位点，有效控制了半导体TiO_2材料的氧化还原能力，提高其在光催化有机合成应用中的选择性，成功用于烯烃的选择性氧化。研究结果表明，通过电子供受体的空间限域，可以实现光生电子空穴的定向分离，从而提高光生电子空穴的分离效率，提高光催化反应效率。
最后，基于稀土上转换发光及能带匹配原理，通过稀土上转换发光材料与半导体材料的有效耦合，构建了能有效利用太阳光谱中紫外、可见和近红外光谱的NaYF_4:Yb~(3+),Er~(3+)@SiO2-CuInS_2光催化体系。该微纳结构光催化剂，能将吸收的980nm的近红外光谱转化为CuInS_2可以充分吸收的540nm可见光，提高了太阳光利用率；通过与光解水制氢耦合，实现了以水氢源高选择性光催化还原CO_2，且避免了牺牲剂的使用；通过具有合适能带的半导体CuInS_2的选择应用，提高了对稀土上转换发光的吸收性能和CO_2的光催化还原的选择性。
本文开展的上述研究工作，对半导体表面的电子供受体的形态、空间位置对微纳结构光催化材料的催化活性的影响机制进行了系统性研究；通过稀土上转换发光材料与半导体材料的有效耦合，将其吸光范围从可见光区拓展到了近红外区。上述微纳结构光催化体系，分别成功应用于水环境中污染物降解、烯烃选择氧化、光催化还原CO_2，取得了令人满意的光催化效果。
Utilization of solar energy is the basic way to solve the energy crisis and environmentpollution by mimicking the photosynthesis existed in nature. Semiconducor materials areproposed as the most promising tools to perform this goal due to their excellent light-electronresponse character. However, they are still suffered from narrow spectral absorbance,recombination of photogenerated electrons and holes and low photocatalytic reaction selectivity,which cause a tardigrade development in the photocatalysis research field. Micro-nanostructurephotocatalyst systems which are usually composed of carrier, electron donor and acceptor (or actas light absorbance), exhibit effective catalytic activity due to wide spectral absorbance andenhanced charge separation. However, the effection on the photocatalytic activity caused by theelectron donors or acceptors morphology has been ignored for a long time.
In this paper, based on the idea of energy up-conversion, morphology controle and spatialconfinement of electron donors and acceptors, we constructed novel micro-nano structurematrials to improve the solar absorbance and charge separation efficiency for the photocatalysis,which were successfully applied in the water water purification, oxidation of olefins and watersplitting.
First, to show the influence caused by the morphology of surface electron donors oracceptors, a new kind of carbonouse TiO_2composite, TiO_2-Cdot, was fabricated as the modelphotocatalyst. It indicated that TiO_2particles strewed with optimal quantity of carbon nanodotshas much higher photoactivity than that of TiO_2overcovered with carbon layer owning to thesufficient exposure of the active sites and efficient separation of photogenerated electrons andholes. According to these results, the different photocatalytic mechanism was discussed. Theestablished mechanism is proposed to be compatible to clarify why the semiconductors modifiedwith other electron acceptors such as metal-semiconductor hybrid materials have the optimalcontents for the photoactivity. Moreover, a piston motion model electrons transfer mechanism was proposed for TiO2@C material for the first time, which maybe has the universality to other kind of core-shell semiconductor hybrid materials with compact shells and need further investigation in the future work.
Second, we prepared a novel photocatalyst, Pt@TiO.2-TCMnPc, based on TiO2nanotube with confinement of electron donor and acceptor at inner and outer surface respectively by a universal method. In which, Pt nanoparticles (electron acceptor) and dye (TCMnPc, electrons donor) are localized at inner and outer surface of a porous TiO2nanotube respectively. The as-designed nanostructure afforded a void space separation state of electron donor and acceptor, which significantly enhanced the charge separation, consequently the catalytic activity for photooxidation of olefins with O2. Moreove, both of the electron donor and acceptor were utilized as active site to activate the substrates by deliberate design avoiding the use of sacrificial agents.
Last, based on the idea of energy up-conversion and band matching, a novel micro-nano structure NaYF4:Yb3+, Er3+@SiO2-CuInS2was fabricated to apply in the photocatalytic water splitting and reduction of CO2. The as-prepared photocatalyst can absorb near infrared light, which improve the utilization efficiency of the solar light. The photocatalytic efficiency and selectivity were remarkably improved.
The results reported in this paper as mentioned aboved should be much helpful to make a rational design on constructure new kind of composite photocatalysts.
在本文中，我们基于表面电子供受体形态控制、电子供受体空间限域、稀土上转换发光等研究策略，通过功能化微纳结构光催化剂的构建，为上述问题的解决提供了新途径。
首先，为了研究表面电子供受体形态对半导体光催化性能的影响，我们构建了具有蛇莓形态的TiO_2-Cdot微纳结构光催化体系，提供了一种TiO_2表面电子供受体碳纳米点的可控合成策略，探讨了碳纳米点分布对TiO_2光催化活性的影响，提出了TiO_2@C核壳结构在光催化过程中可能存在“活塞式”光生电子转移模式。通过对光催化剂吸附性能、光吸收程度、光电响应性能等研究，揭示TiO_2表面碳纳米点的形态是影响微纳结构TiO_2-C组装材料光催化活性的关键因素。
另外，在上述研究二氧化钛和碳复合材料的过程中，我们以碳为还原性物种将TiO_2部分还原，合成出了具有多面体自组装形貌的灰黑色金红石型TiO_2。与普通白色金红石型TiO_2相比，由于Ti3+的存在，使该灰黑色TiO_2具有很强的可见光吸收能力及光电分离能力；在可见光下，其光催化性能显著高于白色金红石型TiO_2和锐钛型P25TiO_2。并且，我们通过二次煅烧钝化TiO_2表面还原态Ti3+，有效提高了灰黑色TiO_2的物理化学稳定性及光催化活性的稳定性。
为了研究表面电子供受体空间位置对半导体光催化性能的影响，我们以TiO_2纳米管为基体，将Pt纳米粒子作为电子受体限域在TiO_2纳米管内部，将兼具光吸收天线和电子供体功能的TCMnPc限域在TiO_2纳米管外部，构建了具有电子供受体空间限域结构的Pt@TiO_2-TCMnPc光催化体系，提供了一种层层组装法和模板法相结合的空间限域微纳结构材料的通用性合成方法。在该微纳结构光催化体系中，电子供、受体作为反应活性位点，有效控制了半导体TiO_2材料的氧化还原能力，提高其在光催化有机合成应用中的选择性，成功用于烯烃的选择性氧化。研究结果表明，通过电子供受体的空间限域，可以实现光生电子空穴的定向分离，从而提高光生电子空穴的分离效率，提高光催化反应效率。
最后，基于稀土上转换发光及能带匹配原理，通过稀土上转换发光材料与半导体材料的有效耦合，构建了能有效利用太阳光谱中紫外、可见和近红外光谱的NaYF_4:Yb~(3+),Er~(3+)@SiO2-CuInS_2光催化体系。该微纳结构光催化剂，能将吸收的980nm的近红外光谱转化为CuInS_2可以充分吸收的540nm可见光，提高了太阳光利用率；通过与光解水制氢耦合，实现了以水氢源高选择性光催化还原CO_2，且避免了牺牲剂的使用；通过具有合适能带的半导体CuInS_2的选择应用，提高了对稀土上转换发光的吸收性能和CO_2的光催化还原的选择性。
本文开展的上述研究工作，对半导体表面的电子供受体的形态、空间位置对微纳结构光催化材料的催化活性的影响机制进行了系统性研究；通过稀土上转换发光材料与半导体材料的有效耦合，将其吸光范围从可见光区拓展到了近红外区。上述微纳结构光催化体系，分别成功应用于水环境中污染物降解、烯烃选择氧化、光催化还原CO_2，取得了令人满意的光催化效果。
Utilization of solar energy is the basic way to solve the energy crisis and environmentpollution by mimicking the photosynthesis existed in nature. Semiconducor materials areproposed as the most promising tools to perform this goal due to their excellent light-electronresponse character. However, they are still suffered from narrow spectral absorbance,recombination of photogenerated electrons and holes and low photocatalytic reaction selectivity,which cause a tardigrade development in the photocatalysis research field. Micro-nanostructurephotocatalyst systems which are usually composed of carrier, electron donor and acceptor (or actas light absorbance), exhibit effective catalytic activity due to wide spectral absorbance andenhanced charge separation. However, the effection on the photocatalytic activity caused by theelectron donors or acceptors morphology has been ignored for a long time.
In this paper, based on the idea of energy up-conversion, morphology controle and spatialconfinement of electron donors and acceptors, we constructed novel micro-nano structurematrials to improve the solar absorbance and charge separation efficiency for the photocatalysis,which were successfully applied in the water water purification, oxidation of olefins and watersplitting.
First, to show the influence caused by the morphology of surface electron donors oracceptors, a new kind of carbonouse TiO_2composite, TiO_2-Cdot, was fabricated as the modelphotocatalyst. It indicated that TiO_2particles strewed with optimal quantity of carbon nanodotshas much higher photoactivity than that of TiO_2overcovered with carbon layer owning to thesufficient exposure of the active sites and efficient separation of photogenerated electrons andholes. According to these results, the different photocatalytic mechanism was discussed. Theestablished mechanism is proposed to be compatible to clarify why the semiconductors modifiedwith other electron acceptors such as metal-semiconductor hybrid materials have the optimalcontents for the photoactivity. Moreover, a piston motion model electrons transfer mechanism was proposed for TiO2@C material for the first time, which maybe has the universality to other kind of core-shell semiconductor hybrid materials with compact shells and need further investigation in the future work.
Second, we prepared a novel photocatalyst, Pt@TiO.2-TCMnPc, based on TiO2nanotube with confinement of electron donor and acceptor at inner and outer surface respectively by a universal method. In which, Pt nanoparticles (electron acceptor) and dye (TCMnPc, electrons donor) are localized at inner and outer surface of a porous TiO2nanotube respectively. The as-designed nanostructure afforded a void space separation state of electron donor and acceptor, which significantly enhanced the charge separation, consequently the catalytic activity for photooxidation of olefins with O2. Moreove, both of the electron donor and acceptor were utilized as active site to activate the substrates by deliberate design avoiding the use of sacrificial agents.
Last, based on the idea of energy up-conversion and band matching, a novel micro-nano structure NaYF4:Yb3+, Er3+@SiO2-CuInS2was fabricated to apply in the photocatalytic water splitting and reduction of CO2. The as-prepared photocatalyst can absorb near infrared light, which improve the utilization efficiency of the solar light. The photocatalytic efficiency and selectivity were remarkably improved.
The results reported in this paper as mentioned aboved should be much helpful to make a rational design on constructure new kind of composite photocatalysts.
引文
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