高分散层状催化剂的制备及其光催化性能研究
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摘要
针对多相催化剂在应用过程中存在的活性组分易团聚、分散度低等问题，本论文以光催化性能为导向，以催化剂活性组分的高分散为切入点，将催化活性金属元素Cr、Ti等引入水滑石(LDHs)层板，实现了原子/亚原子尺度的分散；通过进一步调控粒径尺寸，实现了缺陷位可控的无机纳米催化剂的制备，并在介观尺度进行了多级结构催化剂的组装。采用实验技术和理论计算相结合的手段，对系列LDHs催化剂的晶体结构、能级特征、金属间相互作用进行了深入研究；揭示了催化剂的结构、组成、形貌以及缺陷位等特征对催化性能的影响；发展了一系列可用于光解水制氢(或制氧)、可见光催化以及杀菌等领域的高性能催化剂，为构筑新型高分散催化剂提供了一定的实验及理论基础。
本论文的主要研究内容与结果如下：
1、采用本实验室创制的成核晶化隔离法，将具有可见光吸收性质的Cr元素引入LDHs层板中，合成了MCr–LDHs (M=Cu, Ni, Zn)催化剂，在可见光催化方面展现了良好的性能。CrO_6基元在LDHs介质中的高度分散，导致了MCr–LDHs较窄的禁带宽度，可充分吸收太阳光中的可见光部分，提高了光生载流子的生成效率；LDHs层状结构表面存在大量的OH基团，有助于捕获空穴进而产生自由基，提升了载流子的传输效率。高的载流子生成和分离传输效率是高催化活性的主要原因。该方法可以进一步拓展制备具有可见光响应的氢氧化物或氧化物，有望应用于催化，吸附等领域。
2、基于LDHs层板金属元素高度分散的特点，将TiO_6引入到层板中，获得了MTi–LDHs (M=Ni, Zn, Mg)催化剂，在光分解水制氢方面展现了非常优越的催化性能(314μmol·h~(-1)g~(-1))。结构表征证明了LDHs中TiO_6八面体通过共价键与MO_6(M=Ni, Zn, Mg)八面体相互作用，并呈现高度分散状态。此外，由于MTi–LDHs表面存在大量的缺陷位，相比层状K_2Ti_4O_9可显著降低电子–空穴复合效率。密度泛函计算显示TiO_6和MO_6通过共价作用降低了其禁带宽度，有助于吸收可见光，提高了其光催化性能。这种基于LDHs层板元素高分散的特点，引入相关表面缺陷来制备高性能催化剂，在光解水制氢以及太阳能转化方面具有潜在的应用价值。
3、采用反相微乳液方法，合成了Ti~(3+)掺杂的NiZnTi–LDHs纳米片(4080nm)，表现出优越的可见光分解水制氧性能(2700μmol·h~(-1)g~(-1))及良好的循环稳定性。采用荧光、顺磁共振等手段证实随着LDHs纳米片粒径的减小，表面的Ti3+缺陷位浓度增加；其作为光生电子的受限位降低了电子空穴的复合几率，有效提高了载流子的利用效率，从而表现出优越的可见光催化性能。基于此特征，该材料也表现出良好的可见光抗菌(大肠杆菌、金黄色葡萄球菌、酵母菌)性能。本工作提供了一种通过调变LDHs粒径来调控Ti~(3+)活性位浓度的新方法，从而实现了可见光催化性能的强化，在催化以及太阳能利用方面具有潜在应用价值。
4、以紫藤果实豆荚为模板，采用原子气相沉积(ALD)原位生长焙烧方法，制备了具有优良光催化活性的多级结构ZnAl复合金属氧化物（MMO）。该催化剂从纳米到宏观尺度精确复制了生物模板的多级形貌。相比于利用传统共沉淀法制备的催化剂，利用生物模板获得的MMO催化剂对水中的污染物表现出更强的光催化降解能力。这是由于其形成了多孔状的多级结构，具有高的比表面积和宽的孔径分布。由于生物模板的多样性和LDHs组分的可调性，该多级结构材料在催化、吸附等领域具有广阔应用前景。
5、采用溶胶凝胶原位生长方法，在多种基体(滤纸、海绵、棉质布)表面制备了多级结构LDHs薄膜材料；可以复制不同基体的形貌，该方法可操作性强、成本低、易于大规模制备。该薄膜材料与粉体材料相比(11mg刚果红·g~(-1)LDH)，在水处理吸附染料方面展现了更强的吸附能力(20mg刚果红·g~(-1)LDH)和良好的实际可操作性。本工作提供了一种设计组装新型多级结构LDHs薄膜材料的方法，该类材料可应用于催化、吸附、薄膜分离等领域。
Heterogeneous catalysts generally suffer from serious agglomeration,and low dispersion of active site, which restricts their effective utilization.In this dissertation, the photocatalytic active site was highly dispersed bydistributing the Cr, Ti unit within layered double hydroxides (LDHs)matrix to enhance the efficiency of charge separation and improve thephotoconversion capability. The inorganic nanoparticles with surfaceactive defects were prepared through controlling the particle size. Thehierarchical assemblies were also achieved in micro scale by using thesenanoparticles as building blocks. Both experimental and theoreticalcalculations were carried out to study the crystal structure, energy levelcharacteristics and the interaction of intercalating metals, in order todemonstrate the structure-property correlation. Moreover, the applicationsin splitting water into H_2or O_2, visible-light catalysis, as well asantipathogen performance were explored. This study provided bothexperimental and computational basis for the development of novelhighly-dispersed catalysts.
The main results of this dissertation are as follows:
1. A family of visible-light responsive MCr–LDHs (M=Cu, Ni, Zn)photocatalyst was synthesized by a separate nucleation and aging steps(SNAS), which displays remarkable photocatalytic degradation activityunder visible-light irradiation. The high dispersion of the CrO6unit inthe LDH matrix leads to the lower band gap and the resultingpronounced visible-light absorption. In addition, the abundant OHgroups on the surface of LDH accept photogenerated holes to yieldhighly-reactive hydroxyl radicals, accounting for the excellentphotocatalytic behavior. By virtue of the facile scale-up method and theintrinsic dispersion of the MO6octahedron unit, this approach can beextended for the preparation of other metal hydroxides/oxides for thewidely application in catalysis.
2. Series of photocatalysts for water splitting into hydrogen wereprepared by distributing TiO6unit in a layered MTi–LDHs matrix(M=Ni, Zn, Mg), which displays largely-enhanced H_2–productionphotocatalytic activity (314μmol·h~(-1)g~(-1)) as well as excellent recyclableperformance. Structure measurements reveal that a high dispersion ofTiO6octahedra in the LDH matrix was obtained by the formation ofM~(2+)–O–Ti network, rather different from the aggregation state of TiO6in the inorganic layered material K_2Ti_4O_9. Furthermore, theelectron–hole recombination process was significantly depressed in the Ti-containing LDH materials relative to bulk Ti oxide, which isattributed to the abundant surface defects that serve as trapping sitesfor photogenerated electrons. A theoretical study based on DFTcalculation demonstrates that electronic structure of the TiO6unit wasmodified by adjacent MO6octahedron via covalent interaction,accounting for its superior water splitting behavior. Therefore, thedispersion strategy for TiO6unit within a2D inorganic matrix can beused to enhance the performance in photocatalysis and energyconversion.
3. Ti3+doped NiZnTi-LDH nanosheets with a lateral dimension of4080nm were synthesised using a reverse microemulsion method,which exhibit very high visible-light photocatalytic activity forsplitting water into oxygen (2700μmol·h~(-1)g~(-1)) and antipathogenperformance. The photoluminescence spectra demonstrate that theelectron-hole recombination process was significantly depressed in theLDH nanosheets compared with bulk LDH material, which is attributedto the abundant surface defects serving as trapping sites forphotogenerated electrons. Electron Spin Resonance (ESR)measurement reveals that a high concentration of Ti~(3+)sites aregenerated by creating nanoscized LDH platelets. This work provides afacile method for the preparation of LDH nanosheets containing a highconcentration of Ti3+active sites, which have potential applications in catalysis and solar energy utilization.
4. Hierarchically macro/meso porous mixed metal oxides (MMO)framework with multilevel3D morphologies from nanoscale tomacroscale was fabricated by using a combination of an atomic layerdeposition (ALD) process in situ growth calcination process. It wasfound that the MMO framework can be used as an effective andrecyclable photocatalyst and exhibits higher photocatalytic activitythan the corresponding MMO powdered sample. This is due to thehierarchical structure of the biomorphic MMO framework along with ahigh specific surface area and wide pore size distribution. Our studydemonstrates an exciting approach for enhancing the chemicalperformance of conventional catalysts through biomimicking. It isanticipated that this new strategy can be employed to fabricate variousbio-templated LDH films as well as MMO frameworks.
5. Various LDH films on different substrates (paper, sponge andcloth) were obtained by sol–gel deposition and subsequent in situgrowth procedure, which replicate the morphological properties of thetemplates with advantages of easy manipulation, low-cost, and largesurface area. The obtained films show higher adsorption capacity andexcellent ability to remove dye (20mg·g1LDHCongo Red), comparedwith the corresponding powdered samples (11mg·g1LDHCongo Red).By virtue of the facile sol–gel replication and in situ growth technique, it is expected that a wide variety of LDH films with complicatedmorphologies can be fabricated in a similar way. Therefore, this workprovides new possibilities for the rational design and fabrication ofhierarchical LDH films, which can be potentially applied in the fieldsof catalysts, adsorbents and membrane separation.
本论文的主要研究内容与结果如下：
1、采用本实验室创制的成核晶化隔离法，将具有可见光吸收性质的Cr元素引入LDHs层板中，合成了MCr–LDHs (M=Cu, Ni, Zn)催化剂，在可见光催化方面展现了良好的性能。CrO_6基元在LDHs介质中的高度分散，导致了MCr–LDHs较窄的禁带宽度，可充分吸收太阳光中的可见光部分，提高了光生载流子的生成效率；LDHs层状结构表面存在大量的OH基团，有助于捕获空穴进而产生自由基，提升了载流子的传输效率。高的载流子生成和分离传输效率是高催化活性的主要原因。该方法可以进一步拓展制备具有可见光响应的氢氧化物或氧化物，有望应用于催化，吸附等领域。
2、基于LDHs层板金属元素高度分散的特点，将TiO_6引入到层板中，获得了MTi–LDHs (M=Ni, Zn, Mg)催化剂，在光分解水制氢方面展现了非常优越的催化性能(314μmol·h~(-1)g~(-1))。结构表征证明了LDHs中TiO_6八面体通过共价键与MO_6(M=Ni, Zn, Mg)八面体相互作用，并呈现高度分散状态。此外，由于MTi–LDHs表面存在大量的缺陷位，相比层状K_2Ti_4O_9可显著降低电子–空穴复合效率。密度泛函计算显示TiO_6和MO_6通过共价作用降低了其禁带宽度，有助于吸收可见光，提高了其光催化性能。这种基于LDHs层板元素高分散的特点，引入相关表面缺陷来制备高性能催化剂，在光解水制氢以及太阳能转化方面具有潜在的应用价值。
3、采用反相微乳液方法，合成了Ti~(3+)掺杂的NiZnTi–LDHs纳米片(4080nm)，表现出优越的可见光分解水制氧性能(2700μmol·h~(-1)g~(-1))及良好的循环稳定性。采用荧光、顺磁共振等手段证实随着LDHs纳米片粒径的减小，表面的Ti3+缺陷位浓度增加；其作为光生电子的受限位降低了电子空穴的复合几率，有效提高了载流子的利用效率，从而表现出优越的可见光催化性能。基于此特征，该材料也表现出良好的可见光抗菌(大肠杆菌、金黄色葡萄球菌、酵母菌)性能。本工作提供了一种通过调变LDHs粒径来调控Ti~(3+)活性位浓度的新方法，从而实现了可见光催化性能的强化，在催化以及太阳能利用方面具有潜在应用价值。
4、以紫藤果实豆荚为模板，采用原子气相沉积(ALD)原位生长焙烧方法，制备了具有优良光催化活性的多级结构ZnAl复合金属氧化物（MMO）。该催化剂从纳米到宏观尺度精确复制了生物模板的多级形貌。相比于利用传统共沉淀法制备的催化剂，利用生物模板获得的MMO催化剂对水中的污染物表现出更强的光催化降解能力。这是由于其形成了多孔状的多级结构，具有高的比表面积和宽的孔径分布。由于生物模板的多样性和LDHs组分的可调性，该多级结构材料在催化、吸附等领域具有广阔应用前景。
5、采用溶胶凝胶原位生长方法，在多种基体(滤纸、海绵、棉质布)表面制备了多级结构LDHs薄膜材料；可以复制不同基体的形貌，该方法可操作性强、成本低、易于大规模制备。该薄膜材料与粉体材料相比(11mg刚果红·g~(-1)LDH)，在水处理吸附染料方面展现了更强的吸附能力(20mg刚果红·g~(-1)LDH)和良好的实际可操作性。本工作提供了一种设计组装新型多级结构LDHs薄膜材料的方法，该类材料可应用于催化、吸附、薄膜分离等领域。
Heterogeneous catalysts generally suffer from serious agglomeration,and low dispersion of active site, which restricts their effective utilization.In this dissertation, the photocatalytic active site was highly dispersed bydistributing the Cr, Ti unit within layered double hydroxides (LDHs)matrix to enhance the efficiency of charge separation and improve thephotoconversion capability. The inorganic nanoparticles with surfaceactive defects were prepared through controlling the particle size. Thehierarchical assemblies were also achieved in micro scale by using thesenanoparticles as building blocks. Both experimental and theoreticalcalculations were carried out to study the crystal structure, energy levelcharacteristics and the interaction of intercalating metals, in order todemonstrate the structure-property correlation. Moreover, the applicationsin splitting water into H_2or O_2, visible-light catalysis, as well asantipathogen performance were explored. This study provided bothexperimental and computational basis for the development of novelhighly-dispersed catalysts.
The main results of this dissertation are as follows:
1. A family of visible-light responsive MCr–LDHs (M=Cu, Ni, Zn)photocatalyst was synthesized by a separate nucleation and aging steps(SNAS), which displays remarkable photocatalytic degradation activityunder visible-light irradiation. The high dispersion of the CrO6unit inthe LDH matrix leads to the lower band gap and the resultingpronounced visible-light absorption. In addition, the abundant OHgroups on the surface of LDH accept photogenerated holes to yieldhighly-reactive hydroxyl radicals, accounting for the excellentphotocatalytic behavior. By virtue of the facile scale-up method and theintrinsic dispersion of the MO6octahedron unit, this approach can beextended for the preparation of other metal hydroxides/oxides for thewidely application in catalysis.
2. Series of photocatalysts for water splitting into hydrogen wereprepared by distributing TiO6unit in a layered MTi–LDHs matrix(M=Ni, Zn, Mg), which displays largely-enhanced H_2–productionphotocatalytic activity (314μmol·h~(-1)g~(-1)) as well as excellent recyclableperformance. Structure measurements reveal that a high dispersion ofTiO6octahedra in the LDH matrix was obtained by the formation ofM~(2+)–O–Ti network, rather different from the aggregation state of TiO6in the inorganic layered material K_2Ti_4O_9. Furthermore, theelectron–hole recombination process was significantly depressed in the Ti-containing LDH materials relative to bulk Ti oxide, which isattributed to the abundant surface defects that serve as trapping sitesfor photogenerated electrons. A theoretical study based on DFTcalculation demonstrates that electronic structure of the TiO6unit wasmodified by adjacent MO6octahedron via covalent interaction,accounting for its superior water splitting behavior. Therefore, thedispersion strategy for TiO6unit within a2D inorganic matrix can beused to enhance the performance in photocatalysis and energyconversion.
3. Ti3+doped NiZnTi-LDH nanosheets with a lateral dimension of4080nm were synthesised using a reverse microemulsion method,which exhibit very high visible-light photocatalytic activity forsplitting water into oxygen (2700μmol·h~(-1)g~(-1)) and antipathogenperformance. The photoluminescence spectra demonstrate that theelectron-hole recombination process was significantly depressed in theLDH nanosheets compared with bulk LDH material, which is attributedto the abundant surface defects serving as trapping sites forphotogenerated electrons. Electron Spin Resonance (ESR)measurement reveals that a high concentration of Ti~(3+)sites aregenerated by creating nanoscized LDH platelets. This work provides afacile method for the preparation of LDH nanosheets containing a highconcentration of Ti3+active sites, which have potential applications in catalysis and solar energy utilization.
4. Hierarchically macro/meso porous mixed metal oxides (MMO)framework with multilevel3D morphologies from nanoscale tomacroscale was fabricated by using a combination of an atomic layerdeposition (ALD) process in situ growth calcination process. It wasfound that the MMO framework can be used as an effective andrecyclable photocatalyst and exhibits higher photocatalytic activitythan the corresponding MMO powdered sample. This is due to thehierarchical structure of the biomorphic MMO framework along with ahigh specific surface area and wide pore size distribution. Our studydemonstrates an exciting approach for enhancing the chemicalperformance of conventional catalysts through biomimicking. It isanticipated that this new strategy can be employed to fabricate variousbio-templated LDH films as well as MMO frameworks.
5. Various LDH films on different substrates (paper, sponge andcloth) were obtained by sol–gel deposition and subsequent in situgrowth procedure, which replicate the morphological properties of thetemplates with advantages of easy manipulation, low-cost, and largesurface area. The obtained films show higher adsorption capacity andexcellent ability to remove dye (20mg·g1LDHCongo Red), comparedwith the corresponding powdered samples (11mg·g1LDHCongo Red).By virtue of the facile sol–gel replication and in situ growth technique, it is expected that a wide variety of LDH films with complicatedmorphologies can be fabricated in a similar way. Therefore, this workprovides new possibilities for the rational design and fabrication ofhierarchical LDH films, which can be potentially applied in the fieldsof catalysts, adsorbents and membrane separation.
引文
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