特殊结构氧化铋的液相合成、生长机理与光学性能
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摘要
Bi2O3是一种重要的功能材料，具有宽带隙、高的折射率和介电常数、优良的光电导性和光致发光性能，己被广泛应用于固体氧化物燃料电池、气体传感器、光电材料、高温超导材料、催化剂、功能陶瓷等诸多领域，具有广阔的应用前景。从理论研究和应用方面来说，其简单温和的制备技术及形貌性能的调控都是值得研究的重要课题。在本论文的工作中，采用液相一步沉淀法成功制备出一系列具有不同微结构的Bi2O3，包括斜棱柱状微结构、分等级的花状微结构和连体四面体状微结构，并对不同微结构的生长形成机制进行了深入研究。本论文研究的主要内容和创新点包括以下几个方面：
首先，引入SDBS作为控制剂，在低温(50℃)水相中合成出了高纯度的直径约为2μm、长度为几十微米的一维斜棱柱状α-Bi2O3。通过对反应时间及SDBS用量的考察、分析，提出了定向附着(Oriented attachment)与奥斯特瓦尔德熟化(Ostwald ripening)协同作用的生长机制。同时，研究了样品的光学性能。
其次，在小分子多元醇(丙三醇)协同下，在水热体系中合成出形貌规则、单分散、尺寸为30μm的3D分等级连体花状α-Bi2O3微结构。这种微结构是由宽300nm、厚100nm、端部带尖角的斜棱柱状纳米棒组装而成。在水热反应中，由纳米带，超薄纳米片和斜棱柱状纳米棒等不同构建单元构筑而成的分等级微结构可以在晶体生长的不同阶段获得。通过对α-Bi2O3形态演化的分析，发现在这种独特的分等级微结构的形成过程中存在两种不同类型的自组装—连体花状微结构的自组装和构建单元本身的层层自组装，以此为依据，提出了“两种自组装组合”的形成机制。探讨了丙三醇对连体花状微结构形成的作用，发现其对这种分等级微结构的“中心结点”的形成至关重要。同时对样品的振动特性，光吸收特性和光致发光(PL)特性进行了研究。
然后，在丙三醇体系中，通过改变温度、压力等反应条件，分别在开放体系(90℃)和水热体系(120℃)合成出由十面体和微米棒(两种不同构建单元)构筑而成的相似的分等级花状微结构。详细分析了同一体系(丙三醇体系)，温度和压力影响构建单元形貌及分等级微结构的原因：①影响构建单元形貌的原因：温度和压力的变化改变了丙三醇中的-OH(羟基)与晶体极性晶面的耦合程度，从而改变了α-Bi2O3在[001]方向的生长速率，导致了晶体各向异性的生长。②对分等级微结构的影响：a)在高温和高压下，丙三醇分子优先选择吸附于构建单元，以形成分等级的花状结构。b)空间位阻效应：微米棒的空间位阻远远小于十面体，因而大量的微米棒能够构筑在一起形成花簇(水热体系)，而十面体构筑的花状结构大多是不完整的(开放体系)。样品的光吸收性能和荧光性能由于形貌的不同略显不同。
最后，进行了亚稳态γ-Bi2O3的制备及性能研究工作。在低温(70℃)开放体系，不引入其他氧化物或过渡后离子，只在PEG-400协助下，合成出高温亚稳态的γ-Bi2O3连体四面体。连体四面体微结构通过超薄三角形纳米片的层层自组装构建而成，且γ-Bi2O3的O (氧原子)对“支撑”四面体微结构的构架发挥着重要的作用。体系中NaOH溶液的浓度控制样品的形貌，随着NaOH溶液浓度的增加，样品的形貌由四面体→切边四面体→昆虫状结构。PEG均一有序的长链对产物的相转移起到至关重要的作用，PEG被EG取代，只能合成出α-Bi2O3多面体。与α-Bi2O3的荧光性能比较，归属于晶体表面氧空位(缺陷)的荧光发射谱带在γ-Bi2O3的PL谱图中并没有出现，说明γ-Bi2O3晶体表面的氧空位很少。
通过本论文的研究，得到了具有特殊微结构的α-Bi2O3和γ-Bi2O3微纳米粉体，完善了水热体系和开放体系在水相温和条件下制备特殊微结构Bi2O3的方法。研究的结果将有助于更深入地理解分等级微观结构的形成，也有助于为氧化铋的新型微观结构增添一些有价值的信息。
Bismuth oxide (Bi2O3) is an important functional material with wide band-gap,high refractive index, dielectric permittivity, high oxygen conductivity, remarkablephotoconductivity and photoluminescence. These unique characteristics make Bi2O3suitable for applications in solid oxide fuel cells, sensors, photoelectric materials, hightemperature superconductor materials, functional ceramics and catalysts. Thedevelopment on its simple and mild preparation and morphology-controlled strategyare important topics, which are worthy of study for theoretical research andapplication. In this paper, various Bi2O3microstructures, including oblique prism-like,hierarchical flowerlike and tetrahedral, were synthesized via a one-step solutionprecipitation method. And on the basis of experiment and characterization, we alsodid an in-depth study on the growth and formation mechanisms of each microstructure.The main research results and innovations of the thesis are given in the followingparts.
First,1D oblique prism-like Bi2O3have been synthesized in aqueous-phase atlow temperature and ambient pressure in the presence of sodiumdodecylbenzenesulfonate (SDBS). The oblique prism-like Bi2O3have betterdistribution with an average diameter of2μm and length of up to tens of micrometers.A combined growth mechanism of oriented attachment followed by Ostwald ripeningis proposed for the formation of oblique prism-like Bi2O3. The optical absorption andphotoluminescence (PL) characteristics of the prepared sample were investigated.
Secondly,3D hierarchical siamesed-flowerlike microstructures of α-Bi2O3havebeen synthesized by a glycerin-assisted hydrothermal method. The microflowers of30μm were built up of oblique prism-like nanorobs, with mean width of300nm andthickness of100nm. In the hydrothermal process, hierarchical microstructures constructed by nanoribbons, ultrathin nanoflakes and oblique prism-like nanorobs canbe found at different step of crystal growth. Morphology evolution of α-Bi2O3wasanalyzed and the probable formation mechanism was described as combination of twosteps of self-assembly: layer-by-layer self-assembly of nanoribbons to the obliqueprism-like nanorobs and self-assembly of nanorobs to hierarchicalsiamesed-flowerlike microstructures. Glycerin plays crucial role in the formation ofthe hierarchical structure (the formation of junction). The vibrational properties,optical absorption and photoluminescence (PL) characteristics of the sample wereinvestigated.
Thirdly, we reported a facile solution precipitation method to fabricate the3Dhierarchical flowerlike microstructures of α-Bi2O3composed of decahedrons and rods.How do temperature and pressure affect morphologies of “petals” and flowerlikemicrostructures in the glycerin system?①At90℃and ambient pressure, the OH(hydroxyl radical) of glycerol molecules are more favorably coupled on the polarfaces, which decreases the growth in the [001] direction of α-Bi2O3to formdecahedral shape.②a) At high temperature and pressure, the coupling effect of OHon polar faces is greatly weakened, which leads to an elongation of crystal shape(rod-like shape), and glycerol molecules are more favorably adsorbed on the tip of thepetals to form hierarchical flowerlike structures. b) In addition, steric hindrance ofdecahedron is much higher than robs, which lead to formation of flower clustercomposed of more rods and incomplete flowerlike microstructures composed of a fewdecahedrons. The small difference of optical absorption and photoluminescence (PL)characteristics arises from diversity of morphology.
Finally, we studied the synthesis and property of γ-Bi2O3.Metastable γ-Bi2O3siamesed-tetrahedra have been synthesized at70℃with the assistance of PEG (Mw=400). The obtained tetrahedra are built up of ultrathin triangular nanosheets vialayer-by-layer self-assembly. Oxygen atoms in γ-Bi2O3play critical role inunderpinning tetrahedral structures. The concentration of NaOH solution tunes themorphology and PEG influences not only in the morphology but also in phase transferof sample. Compared with the PL spectrum of α-Bi2O3, the emission peak located around567nm disappears, which are caused by the reduction in crystal defects(oxygen vacancies) of γ-Bi2O3.
In conclusion，distinctive microstructures Bi2O3composed of different buildingblocks are obtained by solution precipitation method. Our findings will help for betterunderstanding of the formation of hierarchical microstructures and will also contributesome valuable information to novel microstructures of Bi2O3.
首先，引入SDBS作为控制剂，在低温(50℃)水相中合成出了高纯度的直径约为2μm、长度为几十微米的一维斜棱柱状α-Bi2O3。通过对反应时间及SDBS用量的考察、分析，提出了定向附着(Oriented attachment)与奥斯特瓦尔德熟化(Ostwald ripening)协同作用的生长机制。同时，研究了样品的光学性能。
其次，在小分子多元醇(丙三醇)协同下，在水热体系中合成出形貌规则、单分散、尺寸为30μm的3D分等级连体花状α-Bi2O3微结构。这种微结构是由宽300nm、厚100nm、端部带尖角的斜棱柱状纳米棒组装而成。在水热反应中，由纳米带，超薄纳米片和斜棱柱状纳米棒等不同构建单元构筑而成的分等级微结构可以在晶体生长的不同阶段获得。通过对α-Bi2O3形态演化的分析，发现在这种独特的分等级微结构的形成过程中存在两种不同类型的自组装—连体花状微结构的自组装和构建单元本身的层层自组装，以此为依据，提出了“两种自组装组合”的形成机制。探讨了丙三醇对连体花状微结构形成的作用，发现其对这种分等级微结构的“中心结点”的形成至关重要。同时对样品的振动特性，光吸收特性和光致发光(PL)特性进行了研究。
然后，在丙三醇体系中，通过改变温度、压力等反应条件，分别在开放体系(90℃)和水热体系(120℃)合成出由十面体和微米棒(两种不同构建单元)构筑而成的相似的分等级花状微结构。详细分析了同一体系(丙三醇体系)，温度和压力影响构建单元形貌及分等级微结构的原因：①影响构建单元形貌的原因：温度和压力的变化改变了丙三醇中的-OH(羟基)与晶体极性晶面的耦合程度，从而改变了α-Bi2O3在[001]方向的生长速率，导致了晶体各向异性的生长。②对分等级微结构的影响：a)在高温和高压下，丙三醇分子优先选择吸附于构建单元，以形成分等级的花状结构。b)空间位阻效应：微米棒的空间位阻远远小于十面体，因而大量的微米棒能够构筑在一起形成花簇(水热体系)，而十面体构筑的花状结构大多是不完整的(开放体系)。样品的光吸收性能和荧光性能由于形貌的不同略显不同。
最后，进行了亚稳态γ-Bi2O3的制备及性能研究工作。在低温(70℃)开放体系，不引入其他氧化物或过渡后离子，只在PEG-400协助下，合成出高温亚稳态的γ-Bi2O3连体四面体。连体四面体微结构通过超薄三角形纳米片的层层自组装构建而成，且γ-Bi2O3的O (氧原子)对“支撑”四面体微结构的构架发挥着重要的作用。体系中NaOH溶液的浓度控制样品的形貌，随着NaOH溶液浓度的增加，样品的形貌由四面体→切边四面体→昆虫状结构。PEG均一有序的长链对产物的相转移起到至关重要的作用，PEG被EG取代，只能合成出α-Bi2O3多面体。与α-Bi2O3的荧光性能比较，归属于晶体表面氧空位(缺陷)的荧光发射谱带在γ-Bi2O3的PL谱图中并没有出现，说明γ-Bi2O3晶体表面的氧空位很少。
通过本论文的研究，得到了具有特殊微结构的α-Bi2O3和γ-Bi2O3微纳米粉体，完善了水热体系和开放体系在水相温和条件下制备特殊微结构Bi2O3的方法。研究的结果将有助于更深入地理解分等级微观结构的形成，也有助于为氧化铋的新型微观结构增添一些有价值的信息。
Bismuth oxide (Bi2O3) is an important functional material with wide band-gap,high refractive index, dielectric permittivity, high oxygen conductivity, remarkablephotoconductivity and photoluminescence. These unique characteristics make Bi2O3suitable for applications in solid oxide fuel cells, sensors, photoelectric materials, hightemperature superconductor materials, functional ceramics and catalysts. Thedevelopment on its simple and mild preparation and morphology-controlled strategyare important topics, which are worthy of study for theoretical research andapplication. In this paper, various Bi2O3microstructures, including oblique prism-like,hierarchical flowerlike and tetrahedral, were synthesized via a one-step solutionprecipitation method. And on the basis of experiment and characterization, we alsodid an in-depth study on the growth and formation mechanisms of each microstructure.The main research results and innovations of the thesis are given in the followingparts.
First,1D oblique prism-like Bi2O3have been synthesized in aqueous-phase atlow temperature and ambient pressure in the presence of sodiumdodecylbenzenesulfonate (SDBS). The oblique prism-like Bi2O3have betterdistribution with an average diameter of2μm and length of up to tens of micrometers.A combined growth mechanism of oriented attachment followed by Ostwald ripeningis proposed for the formation of oblique prism-like Bi2O3. The optical absorption andphotoluminescence (PL) characteristics of the prepared sample were investigated.
Secondly,3D hierarchical siamesed-flowerlike microstructures of α-Bi2O3havebeen synthesized by a glycerin-assisted hydrothermal method. The microflowers of30μm were built up of oblique prism-like nanorobs, with mean width of300nm andthickness of100nm. In the hydrothermal process, hierarchical microstructures constructed by nanoribbons, ultrathin nanoflakes and oblique prism-like nanorobs canbe found at different step of crystal growth. Morphology evolution of α-Bi2O3wasanalyzed and the probable formation mechanism was described as combination of twosteps of self-assembly: layer-by-layer self-assembly of nanoribbons to the obliqueprism-like nanorobs and self-assembly of nanorobs to hierarchicalsiamesed-flowerlike microstructures. Glycerin plays crucial role in the formation ofthe hierarchical structure (the formation of junction). The vibrational properties,optical absorption and photoluminescence (PL) characteristics of the sample wereinvestigated.
Thirdly, we reported a facile solution precipitation method to fabricate the3Dhierarchical flowerlike microstructures of α-Bi2O3composed of decahedrons and rods.How do temperature and pressure affect morphologies of “petals” and flowerlikemicrostructures in the glycerin system?①At90℃and ambient pressure, the OH(hydroxyl radical) of glycerol molecules are more favorably coupled on the polarfaces, which decreases the growth in the [001] direction of α-Bi2O3to formdecahedral shape.②a) At high temperature and pressure, the coupling effect of OHon polar faces is greatly weakened, which leads to an elongation of crystal shape(rod-like shape), and glycerol molecules are more favorably adsorbed on the tip of thepetals to form hierarchical flowerlike structures. b) In addition, steric hindrance ofdecahedron is much higher than robs, which lead to formation of flower clustercomposed of more rods and incomplete flowerlike microstructures composed of a fewdecahedrons. The small difference of optical absorption and photoluminescence (PL)characteristics arises from diversity of morphology.
Finally, we studied the synthesis and property of γ-Bi2O3.Metastable γ-Bi2O3siamesed-tetrahedra have been synthesized at70℃with the assistance of PEG (Mw=400). The obtained tetrahedra are built up of ultrathin triangular nanosheets vialayer-by-layer self-assembly. Oxygen atoms in γ-Bi2O3play critical role inunderpinning tetrahedral structures. The concentration of NaOH solution tunes themorphology and PEG influences not only in the morphology but also in phase transferof sample. Compared with the PL spectrum of α-Bi2O3, the emission peak located around567nm disappears, which are caused by the reduction in crystal defects(oxygen vacancies) of γ-Bi2O3.
In conclusion，distinctive microstructures Bi2O3composed of different buildingblocks are obtained by solution precipitation method. Our findings will help for betterunderstanding of the formation of hierarchical microstructures and will also contributesome valuable information to novel microstructures of Bi2O3.
引文
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