光催化CO₂还原能实现直接利用太阳能将CO₂转化为有机燃料，是降低CO₂浓度解决环境污染问题的绿色方法。以石墨相氮化碳（g-C₃N₄）为首的碳氮材料，拥有横跨CO₂还原和H₂O氧化能级，广泛应用于CO₂还原反应。但是其电子空穴复合率高、活性位点有限、可见光吸收能力差和反应质子提供不足等问题严重限制其光催化还原性能。本论文针对以上局限提出了相应的改进方法，旨在使光催化CO₂还原催化剂更加高效，催化体系更加完善。主要内容包括以下三个方面：

（1）通过引入具有石墨相氮化碳材料相似共轭有机框架的六氮非萘烯类化合物（TPHAP）和三均三嗪基衍生物的三种有机共轭分子构建内建电场，促进电子和空穴的分离效率。研究发现，共轭分子间π-π堆叠作用的增强能够将电子在共轭界面抽离，增强电子空穴分离效率。经过气固相CO₂还原测试，发现复合型催化剂的还原产物CO和CH₄生成效率相比于单一组分催化剂提高数倍。选取界面电荷、能带结构以及共轭结构相互匹配的催化剂构建强内建电场，是合成优异性能催化剂的有效策略。

（2）为探究能带调控对于内建电场强度的影响规律，并解决块状石墨相氮化碳材料比表面积较低，导致活性位点和可见光响应范围有限问题，通过剥离和元素掺杂的方式制备硼掺杂的能带结构可调的超薄石墨相碳氮纳米片（BCN_x），并结合第一章的策略，加入共轭化合物TPHAP，构建系列不同能级差异的异质结构催化剂。研究表明，硼元素掺杂能够有效增强可见光吸收能力，样品BCN₄₀₀的CO平均产率达到7.6 μmol g^-1 h^-1。对能带位置不同的BCNx材料，结合上一章方法，通过静电自组装得到能级匹配最协调的复合催化剂TP/BCN_x。实验证明TP/BCN₄₀₀催化性能显著提高，CO平均产率达到60.3 μmol g^-1 h^-1，有效提升气固相光催化CO₂还原性能。

（3）为解决传统气固和气液固催化模式H₂O和CO₂分子传输能力差，H₂O氧化动力学缓慢导致的光催化CO₂总体性能差的问题。本章引入金属Ag颗粒与石墨相碳氮筑构肖特基结，制备一体式Ag-CN/GOCA气凝胶催化剂，引入苯甲醇氧化反应替代H₂O氧化反应，提出设计介于气-固-液界面的三相的催化模式。经过实验证明，可漂浮三相光催化体系能够有效提升光催化CO₂还原效率，金属Ag纳米颗粒与石墨相碳氮材料形成的肖特基结，能够促进催化界面的电荷快速转移。介于气-固-液界面的三相催化体系，能够同时提升体系中CO₂气体分子扩散及液相苯甲醇分子传质。该方案通过促进氧化端半反应驱动还原端CO₂分子的还原，使还原产物生成速率提升6.3倍，能够从催化体系上解决可见光驱动光催化还原CO₂活性低的问题。

      Photocatalytic CO₂ reduction can convert CO₂ into organic fuel derived by solar energy, which is a green method to reduce CO₂ concentration and solve environmental pollution problems. Graphitic carbon nitride (g-C₃N₄), have been widely used in CO₂ reduction reactions due to their cross-energy levels of CO₂ reduction and H₂O oxidation. However, its photocatalytic reduction performance is seriously limited by its high electron-hole recombination rate, limited active sites, poor visible light absorption capacity and insufficient supply of protons. In this paper, the corresponding improvement methods are proposed for the above limitations, aiming to make the photocatalytic CO₂ reduction catalyst more efficient and the catalytic system more perfect. The main contents include the following three aspects:

       (1) The built-in electric field is constructed by introducing three catalysts of 2,5,8-tri(4'-pyridyl)-1,3,4,6,7,9-hexaazaphenalene (TPHAP) and tri-s-triazine derivatives with similar conjugated organic frameworks of graphitic carbon nitride materials to promote the separation rate of electrons and holes. It is found that the enhancement of π-π stacking interaction between conjugated molecules can extract electrons from the conjugated interface and enhance the separation efficiency of electron-hole. It was found that the reduction product CO and CH₄ generation efficiency of the composite catalyst was several times higher than that of the single component catalyst based on the gas-solid mode. This work provides a novel strategy for improving CO₂ photoreduction through controlling the interface charge, energy band structure and the total.

        (2) For further understanding the relationship between the band structures of heterojunction and built-in electric filed, boron-doped ultra-thin graphite phase carbonitride nanosheets (BCN_x) with adjustable band structure were prepared by exfoliation and element doping, which could also solve the problem that the low specific surface area of bulk carbon nitride materials leads to limited active sites and visible light response range. Combined with the strategy of the first chapter, the conjugated compound TPHAP was added to construct a series of heterostructure catalysts with different energy level differences. Studies have shown that boron doping can effectively enhance the visible light absorption capacity and increase the active sites. The average CO yield of the sample BCN₄₀₀ reaches 7.6 μmol g^-1 h^-1. By adjusting the energy band position of BCN_x material, the most coordinated composite catalyst TP/BCN₄₀₀ with energy level matching was obtain-ed by electrostatic self-assembly using the method in the previous chapter. The experimental results show that the catalytic performance is significantly improved, and the average yield of CO reaches 60.3 μmol g^-1 h^-1, which effectively improves the photocatalytic CO₂ reduction performance of gas-solid phase.

        (3) The traditional gas-solid and gas-liquid-solid mode for CO₂ photoreduction present drawbacks of poor transport capacity of H₂O and CO₂ molecular and sluggish kinetics of H₂O oxidation reaction, resulting in poor photocatalytic CO₂ reduction performance. In order to solve above problems, the integrated Ag-CN/GOCA aerogel catalysts in three-phase reaction mode were prepared by introducing the Schottky junction between metal Ag particles and graphitic carbon nitrogen, and replacing H₂O oxidation by reactive benzyl alcohol oxidation reaction. It was experimentally proved that the floatable three-phase photocatalytic system can effectively enhance the photocatalytic CO₂ reduction efficiency, and the Schottky junction formed by metal Ag nanoparticles and graphitic carbon nitrogen can promote rapid charge separation and transfer at the catalytic interface. The three-phase catalytic system mediated at the gas-solid-liquid interface can simultaneously enhance the diffusion of CO₂ gas molecules and the molecular mass transfer of liquid-phase benzyl alcohol in the system. above strategy effectively enhance the CO₂ photoreduction performance by promoting the oxidation half-reaction, which can increase the rate of the reduction product generation by 6.3 times, and can solve the problem of low activity of visible-light-driven photocatalytic reduction of CO₂ in terms of catalytic system.

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