磷基纳米复合材料的制备及其催化性能研究
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摘要
环境污染和能源问题目前仍是困扰人类可持续发展的难题。近年来,磷基复合纳米材料在环境保护和清洁能源开发等方面显示出广泛的应用前景,已成为纳米科学领域的研究热点之一。利用液相法合成磷基纳米材料具有操作简单、效率高、适用范围广、合成颗粒质量好等优点,在合成中广为采用。然而,寻找一种简单方便的液相合成法实现微纳米材料尺寸、结构、形貌,尤其是具有特定晶面、特定取向的功能微纳米晶的可控合成仍是一个巨大的挑战。本课题以磷基复合材料作为研究对象,探索氟羟基磷灰石(FHAp)、银、Ag/FHAp以及Ag@Ag3PO4等几种磷基纳米材料的液相法可控制备。主要研究结果如下：
(1)以EDTA和柠檬酸(CA)混合螯合剂作为有机修饰剂,通过改变反应条件,制备了一系列新颖形貌和结构的FHAp微纳米晶体,包括：具有高比例(0001)晶面的六方微米花,六方微米梭,六方柱,二十面体,六方微纳米棒等特殊微纳米结构。研究了反应体系的pH值、两种螯合剂的用量、氟离子的用量以及水热时间温度等因素对产品颗粒微结构的影响。弱酸性介质有利于具有规则形貌FHAp晶体的生长,碱性介质则有利于FHAp一维不规则纳米结构如纳米棒和纳米晶须的合成。通过控制Ca/EDTA摩尔比,FHAp产物的形貌由三维多晶自组装结构逐渐演变到一维单晶纳米结构。在此基础上,简单地控制所使用CA或氟离子的用量,实现了对一维FHAp六方微纳米晶体的形貌和尺寸的控制。氟离子对于具有规则形貌的一维FHAp六方形微纳米晶体的生成中起到了关键的作用。
(2)展示了一种简单易行一步法水热合成FHAp中空微纳米材料。以EDTA和CA作为晶体生长控制剂,通过改变NaF前躯体的加入顺序,成功地合成出了几种具有规则几何外形以及分级FHAp中空微纳米结构。通过改变水热温度和反应初始溶液pH,实现了对FHAp中空微纳米颗粒形貌的调控。机理研究表明,具有规则几何外形的FHAp中空微纳米颗粒的形成可能与CaF2颗粒充当原位模板有关,Ostwald熟化机制可以用来解释FHAp分级中空微米结构的形成。此外,其他反应条件,例如螯合剂的用量,也可能是促使FHAp中空微纳米结构形成的重要因素。
(3)利用EDTA作为螯合剂和还原剂,一步水热合成出FHAp微晶负载纳米银Ag/FHAp复合材料。HAp载体微粒尺寸在1-2μm之间,负载纳米Ag颗粒平均尺寸约为30 nm,分散性较好。通过改变AgN03前躯体使用量,合成出不同银负载量和尺寸的Ag/FHAp复合纳米材料。pH值对于Ag/FHAp复合纳米结构的形成起到了关键的作用,通过改变反应初始溶液的pH值,不仅可以调控FHAp载体微粒的形貌,还可以改变纳米银的负载量。紫外-可见吸收光谱分析表明所合成的不同纳米银负载量的Ag/FHAp复合纳米材料具有特征的银纳米颗粒的等离子共振吸收峰。
(4)以EDTA为还原剂和螯合剂,水热制备出了亚微米级银颗粒。所合成的亚微米级银颗粒尺寸在200-500 nm之间,分散性较好。通过不同水热时间的样品形貌分析,发现该实验条件所得出的亚微米级银颗粒可能由纳米级银晶体聚集生长而成。通过改变水热反应时间,实现了亚微米级银颗粒的形貌和尺寸的可控。研究了所合成的亚微米级银颗粒催化硼氢化钠还原硝基苯酚反应的活性,结果表明,所合成的亚微米级银颗粒对该反应具有良好的催化活性。
(5)通过沉淀法和光化学还原法制备出Ag@Ag3PO4复合纳米结构。制得的Ag@Ag3PO4复合光催化剂在可见光区域具有明显的吸收,光吸收阈值延伸到550 nm左右,表明其在可见光下具有潜在的光催化活性。利用罗丹明B评价了表面等离子体光催化材料降解有机物的催化活性。Ag@Ag3PO4复合光催化剂具有极高的可见光光催化活性,数分钟内罗丹明B时脱色率已接近100%,其光催化活性是氮掺杂的二氧化钛活性的数十倍。Ag@Ag3PO4高光催化活性可能与Ag3PO4舌性高以及纳米银具有表面等离子体共振吸收性质有关。重复使用实验表明Ag@Ag3PO4具有良好的稳定性。
Enviromnent and energy issues are still the bottleneck for the continuable development of human being. Nowadays, phosphorus-based nanocomposites have been attracted great interest in environmental protection and clean energy field. Solution-based methods have been intensively used in the syntheis of phosphorus-based nanomaterials, owing to its simplicity, effective, feasible, and versatility. Still, it remains a significant challenge to access micro-/nanomaterials with the controllable size, morphology, especially, the crystal factes or growth orientation. In this work, we developed some novel and easy solution-based mehods for the controlled-synthesis of phosphorus-based nanocomposites, such as F-substituted hydroxyapatite (FHAp), Ag/FHAp, and Ag@Ag3PO4. The details are as follows:
(1) A facile strategy for the shape-controlled synthesis of FHAp microcrystals based upon using a combination of EDTA and citric acid (CA) was demonstrated. Novel, well-defined FHAp microcrystals of various shapes, such as hexagonal disks with predominant (0001) faces, hexagonal shuttles, hexagonal prisms, icosahedrons, and hexagonal microrods, were fabricated. The effects of the solution pH value, amount of chelating reagents and fluride ions and hydrothermal time and temperature were investigated in detail. It was found that the acidic medium is benifical for the formation of one-dimensional FHAp microstructures, while the basic reaction soluition favors the yield of three-dimensional (3D) FHAp microstructures. In this double-chelating-agent system, careful control over the Ca/EDTA molar ratio enabled a fine control over the morphology of FHAp particles from 3D polycrystalline microstructures to ID well-faceted single-crystal microrods. Based on this result, simply varying the concentration of CA and/or fluoride ions could allowe the shape-and size-control over 1D well-faceted FHAp microcrystals. F- ions were found to play a critical role in the formation of well-defined hexagonal microcrystals.
(2) A facile single-step hydrothermal method was developed for the synthesis of FHAp hollow micro-/nanostructures. By using EDTA and CA as mixed chelating reagents and simple variation of F- ions addition order, FHAp hollow micro-/nanostructures with well-defined morphologies, including hollow hexagonal rods, hexagonal prisms, and hierarchical microstructures were synthesized in single step. It was found that CaF2 particles formed most likely acted as the in situ template for the formation of hollow FHAp crystals. Time-dependent experimental results indicated that Ostwald ripening process could be used to explain the formation mechanism of the hierarchical hollow FHAp microparticles. In addition, it is believed that other factors, for example, hydrothermal condition and chelating reagent, may promote the formation of hollow FHAp particles.
(3) Silver-fluorapatite composite which consists of fluorapatite microcrystals (FHAp MPs) decorated with silver nanoparticles (Ag NPs) were prepared through a facile single-step hydrothermal method. The synthesis process involves the use of EDTA as both a chelating agent and a reducing agent, allowing the one-pot formation of Ag/FHAp composites. The Ag NPs prepared via this method exhibit monodispersed size distribution, around 30 nm, and essentially uniform dispersion on FHAp MPs supports with sizes of 1-2μm. We demonstrated that the population and size of Ag NPs in the Ag/FHAp composites can be tuned easily by varying the concentration of silver nitrate in the starting reaction solution, as well as by varying the pH value of solution. Additionally we also demonstrated that the resulting Ag/FHAp composites with different Ag loadings possess tunable surface plasmon resonance properties.
(4) A facile, efficient, and environmentally friendly synthetic route was developed to fabricate silver submicron-sized particles by reducing silver nitrate with EDTA in aqueous solution. It was found that by varying the amount of EDTA utilized in the reaction medium and/or hydrothermal reaction time, the size of prepared silver particles can be readily controlled from 200 to 500 nm. Compared with silver nanoparticles, the as-synthesized submicron-sized silver particles were found to show a comparable catalytic activity towards the reduction of 4-nitrophenol to 4-aminophenol in the presence of an excess amount of NaBH4.
(5) Novel Ag@Ag3PO4 composite photocatalysts were prepared by a simple precipitation and photoreduction methods. The as-prepared photocatalysts can absorb solar energy with a wavelength shorter than 550 nm. The photocatalytic activity of as-prepared samples was evaluated by photocatalytic decolorization of Rhodamine B (RhB) aqueous solution at ambient temperature under visible-light irradiation. The prepared Ag@Ag3PO4 composite photocatalysts exhibits an excellent visible-light photocatalytic activity for photocatalytic degradation of RhB in water, and their photocatalytic activity exceeds that of nitrogen-doped TiO2 by a factor of more than 10. The mechanism suggests that the high photocatalytic activity and excellent stability may result from the super sensitivity of Ag3PO4 to light and the surface plasmon resonance of Ag nanoparticles in the region of visible light. The composite photocatalysts maintain a high level even though used for five times.
(1)以EDTA和柠檬酸(CA)混合螯合剂作为有机修饰剂,通过改变反应条件,制备了一系列新颖形貌和结构的FHAp微纳米晶体,包括：具有高比例(0001)晶面的六方微米花,六方微米梭,六方柱,二十面体,六方微纳米棒等特殊微纳米结构。研究了反应体系的pH值、两种螯合剂的用量、氟离子的用量以及水热时间温度等因素对产品颗粒微结构的影响。弱酸性介质有利于具有规则形貌FHAp晶体的生长,碱性介质则有利于FHAp一维不规则纳米结构如纳米棒和纳米晶须的合成。通过控制Ca/EDTA摩尔比,FHAp产物的形貌由三维多晶自组装结构逐渐演变到一维单晶纳米结构。在此基础上,简单地控制所使用CA或氟离子的用量,实现了对一维FHAp六方微纳米晶体的形貌和尺寸的控制。氟离子对于具有规则形貌的一维FHAp六方形微纳米晶体的生成中起到了关键的作用。
(2)展示了一种简单易行一步法水热合成FHAp中空微纳米材料。以EDTA和CA作为晶体生长控制剂,通过改变NaF前躯体的加入顺序,成功地合成出了几种具有规则几何外形以及分级FHAp中空微纳米结构。通过改变水热温度和反应初始溶液pH,实现了对FHAp中空微纳米颗粒形貌的调控。机理研究表明,具有规则几何外形的FHAp中空微纳米颗粒的形成可能与CaF2颗粒充当原位模板有关,Ostwald熟化机制可以用来解释FHAp分级中空微米结构的形成。此外,其他反应条件,例如螯合剂的用量,也可能是促使FHAp中空微纳米结构形成的重要因素。
(3)利用EDTA作为螯合剂和还原剂,一步水热合成出FHAp微晶负载纳米银Ag/FHAp复合材料。HAp载体微粒尺寸在1-2μm之间,负载纳米Ag颗粒平均尺寸约为30 nm,分散性较好。通过改变AgN03前躯体使用量,合成出不同银负载量和尺寸的Ag/FHAp复合纳米材料。pH值对于Ag/FHAp复合纳米结构的形成起到了关键的作用,通过改变反应初始溶液的pH值,不仅可以调控FHAp载体微粒的形貌,还可以改变纳米银的负载量。紫外-可见吸收光谱分析表明所合成的不同纳米银负载量的Ag/FHAp复合纳米材料具有特征的银纳米颗粒的等离子共振吸收峰。
(4)以EDTA为还原剂和螯合剂,水热制备出了亚微米级银颗粒。所合成的亚微米级银颗粒尺寸在200-500 nm之间,分散性较好。通过不同水热时间的样品形貌分析,发现该实验条件所得出的亚微米级银颗粒可能由纳米级银晶体聚集生长而成。通过改变水热反应时间,实现了亚微米级银颗粒的形貌和尺寸的可控。研究了所合成的亚微米级银颗粒催化硼氢化钠还原硝基苯酚反应的活性,结果表明,所合成的亚微米级银颗粒对该反应具有良好的催化活性。
(5)通过沉淀法和光化学还原法制备出Ag@Ag3PO4复合纳米结构。制得的Ag@Ag3PO4复合光催化剂在可见光区域具有明显的吸收,光吸收阈值延伸到550 nm左右,表明其在可见光下具有潜在的光催化活性。利用罗丹明B评价了表面等离子体光催化材料降解有机物的催化活性。Ag@Ag3PO4复合光催化剂具有极高的可见光光催化活性,数分钟内罗丹明B时脱色率已接近100%,其光催化活性是氮掺杂的二氧化钛活性的数十倍。Ag@Ag3PO4高光催化活性可能与Ag3PO4舌性高以及纳米银具有表面等离子体共振吸收性质有关。重复使用实验表明Ag@Ag3PO4具有良好的稳定性。
Enviromnent and energy issues are still the bottleneck for the continuable development of human being. Nowadays, phosphorus-based nanocomposites have been attracted great interest in environmental protection and clean energy field. Solution-based methods have been intensively used in the syntheis of phosphorus-based nanomaterials, owing to its simplicity, effective, feasible, and versatility. Still, it remains a significant challenge to access micro-/nanomaterials with the controllable size, morphology, especially, the crystal factes or growth orientation. In this work, we developed some novel and easy solution-based mehods for the controlled-synthesis of phosphorus-based nanocomposites, such as F-substituted hydroxyapatite (FHAp), Ag/FHAp, and Ag@Ag3PO4. The details are as follows:
(1) A facile strategy for the shape-controlled synthesis of FHAp microcrystals based upon using a combination of EDTA and citric acid (CA) was demonstrated. Novel, well-defined FHAp microcrystals of various shapes, such as hexagonal disks with predominant (0001) faces, hexagonal shuttles, hexagonal prisms, icosahedrons, and hexagonal microrods, were fabricated. The effects of the solution pH value, amount of chelating reagents and fluride ions and hydrothermal time and temperature were investigated in detail. It was found that the acidic medium is benifical for the formation of one-dimensional FHAp microstructures, while the basic reaction soluition favors the yield of three-dimensional (3D) FHAp microstructures. In this double-chelating-agent system, careful control over the Ca/EDTA molar ratio enabled a fine control over the morphology of FHAp particles from 3D polycrystalline microstructures to ID well-faceted single-crystal microrods. Based on this result, simply varying the concentration of CA and/or fluoride ions could allowe the shape-and size-control over 1D well-faceted FHAp microcrystals. F- ions were found to play a critical role in the formation of well-defined hexagonal microcrystals.
(2) A facile single-step hydrothermal method was developed for the synthesis of FHAp hollow micro-/nanostructures. By using EDTA and CA as mixed chelating reagents and simple variation of F- ions addition order, FHAp hollow micro-/nanostructures with well-defined morphologies, including hollow hexagonal rods, hexagonal prisms, and hierarchical microstructures were synthesized in single step. It was found that CaF2 particles formed most likely acted as the in situ template for the formation of hollow FHAp crystals. Time-dependent experimental results indicated that Ostwald ripening process could be used to explain the formation mechanism of the hierarchical hollow FHAp microparticles. In addition, it is believed that other factors, for example, hydrothermal condition and chelating reagent, may promote the formation of hollow FHAp particles.
(3) Silver-fluorapatite composite which consists of fluorapatite microcrystals (FHAp MPs) decorated with silver nanoparticles (Ag NPs) were prepared through a facile single-step hydrothermal method. The synthesis process involves the use of EDTA as both a chelating agent and a reducing agent, allowing the one-pot formation of Ag/FHAp composites. The Ag NPs prepared via this method exhibit monodispersed size distribution, around 30 nm, and essentially uniform dispersion on FHAp MPs supports with sizes of 1-2μm. We demonstrated that the population and size of Ag NPs in the Ag/FHAp composites can be tuned easily by varying the concentration of silver nitrate in the starting reaction solution, as well as by varying the pH value of solution. Additionally we also demonstrated that the resulting Ag/FHAp composites with different Ag loadings possess tunable surface plasmon resonance properties.
(4) A facile, efficient, and environmentally friendly synthetic route was developed to fabricate silver submicron-sized particles by reducing silver nitrate with EDTA in aqueous solution. It was found that by varying the amount of EDTA utilized in the reaction medium and/or hydrothermal reaction time, the size of prepared silver particles can be readily controlled from 200 to 500 nm. Compared with silver nanoparticles, the as-synthesized submicron-sized silver particles were found to show a comparable catalytic activity towards the reduction of 4-nitrophenol to 4-aminophenol in the presence of an excess amount of NaBH4.
(5) Novel Ag@Ag3PO4 composite photocatalysts were prepared by a simple precipitation and photoreduction methods. The as-prepared photocatalysts can absorb solar energy with a wavelength shorter than 550 nm. The photocatalytic activity of as-prepared samples was evaluated by photocatalytic decolorization of Rhodamine B (RhB) aqueous solution at ambient temperature under visible-light irradiation. The prepared Ag@Ag3PO4 composite photocatalysts exhibits an excellent visible-light photocatalytic activity for photocatalytic degradation of RhB in water, and their photocatalytic activity exceeds that of nitrogen-doped TiO2 by a factor of more than 10. The mechanism suggests that the high photocatalytic activity and excellent stability may result from the super sensitivity of Ag3PO4 to light and the surface plasmon resonance of Ag nanoparticles in the region of visible light. The composite photocatalysts maintain a high level even though used for five times.
引文
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