氧化铟、硫化铟纳米结构材料的液相合成及性质研究
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摘要
本论文主要探讨了利用液相化学法控制合成Ⅲ-Ⅵ族半导体化合物—氧化铟(In_2O_3)和硫化铟(β-In_2S_3)纳米结构材料。分别从材料制备、形成机制、以及性质表征和应用研究三个方面进行了论述,内容涉及亚稳相刚玉结构In_2O_3纳米片的合成、形成机制、光催化性质;非水介质中立方相In_2O_3纳米立方块的控制合成、光学性质、以纳米立方块为基本构筑单元的层层自组装薄膜的制备及光学性质;花状氧化铟纳米级次结构材料的合成、形成机制、光学性质;β-In_2S_3纳米管的制备、形成机制以及光催化性质;氧化铟纳米颗粒及纳米带的水热/溶剂热合成与表征等。通过对In_2O_3和β-In_2S_3纳米结构材料的控制合成和性质表征以及性能方面的研究,旨在探索液相体系中纳米结构材料形成的内在机制,寻找纳米结构材料控制合成更加有效的手段和途径。
1.溶液法一步合成刚玉型亚稳相三氧化二铟:前驱体对产品物相的影响
利用乙醇溶剂热方法,在较低温度200℃,首次一步直接合成了六方结构的In_2O_3(H-In_2O_3)六边形纳米片。纳米片边长为100-200nm,厚度约为30nm。在甲醇/水存在下,90℃的加热干燥过程中相对较弱键断裂,释放出少量乙酰丙酮配体,即释放出的acac~-,为了平衡电荷,acac~-夺取甲醇分子中的质子形成Hacac分子。生成的甲氧基负离子则占据acac~-让出的空轨道,生成铟离子与甲氧基和乙酰丙酮混和配体配位的配合物。我们通过X射线粉末衍射(XRD)、红外(IR)、热重分析(TGA)、核磁共振(NMR)、X射线光电子能谱(XPS)等技术对此配合物进行了表征,这些表征结果表明配合物分子中存在着少量的甲氧基(-OCH_3)基团。以此配合物为前驱体进行乙醇溶剂热反应,即得到刚玉型亚稳相氧化铟。而乙酰丙酮铟为前驱体的溶剂热反应得到的为立方相的氧化铟(C-In_2O_3)。
为深入理解前驱体的微小差异影响最终产物氧化铟物相的机制,我们通过XRD、IR技术对实验过程进行了跟踪,并对反应上清液进行了~(13)C NMR及~1HNMR分析。结果表明,C-In_2O_3的生成是通过乙酰丙酮铟的简单热分解,而H-In_2O_3则是由于前驱体配合物的水解所得。前驱体间微小的差异导致不同的反应机理进而形成不同物相产物,这在以往的科研工作中经常被忽视。所合成的六方相氧化铟纳米晶与立方相氧化铟以及Degussa P25相比,有着更强的催化降解苯酚的能力。
2.三氧化二铟纳米立方块的合成及其自组装膜
以乙酰丙酮铟为前驱体,在不同的有机溶剂中进行溶剂热反应,得到表面平滑,棱角规则清晰的立方三氧化二铟纳米立方块。反应溶剂由乙醇改变为n-丁醇、n-辛醇、苯,得到的纳米立方块边长从约21nm减小到约12nm、8nm和6nm,厚度从8nm减小到约6nm,5nm和3nm。
在不同溶剂中得到的不同尺寸的氧化铟纳米晶均在可见光区有四个强的发射峰,其中心分别位于451nm(蓝色)、548、568nm(黄色)和616nm(橙色)。这说明样品中含有丰富的氧空位,产生了不同的能级,这样在光激发的过程中使紫外带边发射(NBE)与深能级发射(DL)的比值非常小,因此导致光致发光(PL)光谱上出现四个可见光发射峰。
采用层层自组装技术,将氧化铟无机纳米颗粒自组装成膜。原子力显微镜(AFM)表征表明薄膜表面颗粒分布紧密均匀,单层膜的厚度为6.39-15.15nm。我们利用紫外可见吸收光谱记录了多层膜制备过程,即监测了每次沉积循环后所形成的薄膜的吸收光谱。随着沉积循环次数的增加,薄膜吸收峰的强度近线性增强,这为多层膜组装,厚度逐渐增长提供了证据。同时随沉积循环次数增多,膜的厚度增加,其荧光发光强度呈线性增强。
3.纳米花状In_2O_3级次纳米结构的制备、表征及光学性质
利用乙酰丙酮铟为前驱体,甲苯溶剂热方法制备了具有级次结构的新型花状立方氧化铟,纳米花由粒径为3-5nm的纳米颗粒组成。通过XRD、FT-IR、TEM、HR-TEM等技术对其进行了表征。
由于乙酰丙酮化合物的热分解速度很慢,氧化铟纳米晶生长的速度较慢。在这种情况下,纳米小颗粒之间碰撞聚集的速度要大于纳米晶生长的速度,生成的氧化铟纳米颗粒为了降低其表面能量,开始随意聚集,这样纳米颗粒的聚集体就会渐渐形成。随着反应时间的延长,氧化铟纳米颗粒逐渐聚集形成花状纳米结构。
这种In_2O_3花状纳米结构具有独特的发光性质,发射中心分别处于438nm(蓝)、546nm、569nm(黄)、618nm(橙)处。蓝光和黄色光应归因于光子激发的空穴和占据氧空位的电子的复合。而位于618nm的发射则是由InO_6八面体中的缺陷造成的。
4.硫化铟纳米管的溶剂热合成、表征及其光学性能研究
以硝酸铟In(NO_3)_3·4H_2O作铟源,十二硫醇作硫源,通过吡啶溶剂热反应一步得到β-In_2S_3纳米管。纳米管两端封闭,外径约为10-20nm,管壁厚约2nm,长度达到微米级。HR-TEM照片表明纳米管由β-In_2S_3纳米颗粒无序组装而成。
我们通过TEM、FESEM、XRD、IR、TG、元素分析等手段对在不同时间获得的产品进行了表征,提出了纳米管的形成机制。即In~(3+)在体系中水解首先生成铟的氢氧化物,硫醇在溶剂热条件下分解释放出S~(2-),体系中溶解的In~(3+)与S~(2-)反应并发生异相成核生成硫化铟,同时随反应的进行铟的氢氧化物不断溶解,所形成的硫化铟纳米颗粒聚集成纳米片状结构,纳米片状结构在240℃,一定压力下,发生卷曲形成纳米管。所制备的硫化铟纳米管有着比P25更好的催化降解罗丹明B的能力。
5.氧化铟纳米颗粒及纳米带的合成与表征
在溶剂热体系中,我们利用In(NO_3)_3·4H_2O作为铟源,通过调节体系的含水量来控制铟盐的水解反应,以达到控制产物物相及其形貌的目的。乙醇溶剂热反应体系中,铟盐水解生成In(OH)_3,In(OH)_3然后进一步脱水形成In_2O_3晶粒。In(OH)_3向In_2O_3的相转变可以理解为“溶解-再结晶”机制,而In_2O_3比In(OH)_3具有更低的溶解度则为其驱动力。而在水热体系中,铟离子充分水解,由于油酸钠水溶液适宜的碱度提供了更多的氢氧根离子,促进了In(OH)_3纳米晶的定向生长,得到了纳米带结构的In(OH)_3。进一步在300℃下进行热处理后,即可得到立方相氧化铟单晶纳米带。
UV-vis吸收光谱中,In_2O_3纳米颗粒和纳米带的分别在273,323nm处有强吸收,较块体In_2O_3的UV光谱有大的蓝移,这是弱的量子限域效应所引起的。所合成的氧化铟纳米颗粒及纳米带的室温光致发光光谱有着明显不同,这是由于经过不同的合成路线制备的纳米结构氧化铟具有不同的缺氧状态。
This paper is focused on the controlled synthesis of indium oxide(In_2O_3) and indium sulfide(In_2S_3) nanostructures,n-type semiconducting oxide ofⅢ-Ⅵcompounds,through solution-phase chemistry routes.Investigations are based on three aspects:controlled synthesis,formation mechanisms,and properties and applications.The contents mainly include metastable corundum-type In_2O_3 nanoplates' preparation,the effects of precursors on the products,formation mechanism and photocatalytic properties;the cubic In_2O_3 nanocubes' preparation, size-controlling,the film of the nanocuboids fabricated onto various substrates via layer by layer self-assembly technique and their optical properties;fabrication of Indium oxide with flowerlike hierarchical structure;synthesis of ultra thin tetragonalβ-in_2S_3 nanotubes,formation mechanism,optical and photocatalytic properties; synthesis and characterization of In_2O_3 nanoparticles and nanobelts via hydro/solvothermal routes.Through In_2O_3 and In_2S_3 nanocrystals' preparation, size-controlling,formation mechanisms and optical and photocatalytic properties,we intend to study the intrinsic controlling mechanism of the nanocrystal formation and look for more effective ways to synthesis of nanostructural materials.
1.Direct solution synthesis of corundum-type In_2O_3:effects of precursors on products
Nanostructured metastable corundum-type In_2O_3 was directly synthesized by a low temperature solvothermal method.The as-prepared products were characterized by X-ray diffractions(XRD),Scan Electron Microscopy(SEM),Transmission Electron Microscopy(TEM) and Fourier Transform Infrared(FT-IR) spectrum in detail. H-In_2O_3 nanoparticles exhibit as hexagonal nanoplates with a side length of 100-200 nm and a thickness of ca.30 nm.The effects of precursors on the products were investigated.It is proposed that the existence of-OCH_3 in the H-In_2O_3 precursor leads to a hydrolysis process rather than thermal decomposition to form the H-In_2O_3. Gas-Chromatography(GC) and Nuclear Magnetic Resonance Spectrum(NMR) of reaction solutions also reveal that the formation of the C-In_2O_3 only goes through the simple thermal decomposition of Ln(acac)_3,while the hydrolysis is the main process during the formation of H-In_2O_3.The present direct solution preparation provides a low-temperature route to H-In_2O_3 and there is no crystalline intermediate during the formation of H-In_2O_3.Moreover,the H-In_2O_3 exhibited higher photocatalytic activity for the degradation of phenol than C-In_2O_3 nanocubes and commercial Degussa P25.
2.Synthesis of In_2O_3 nanocuboids and the corresponding self-assembled films
In_2O_3 nanocuboids have been solvothermally synthesized using indium acetylacetonate as precursor.The size of the nanocuboids could be tunable by adjusting the solvent.The particle sizes of the products obtained from ethanol, n-buthanol,n-octanol and benzene are respectively 21,12,8,6 nm.The PL(all the samples excited at 330 nm,room temperature) emission behaviors of the In_2O_3 nanocrystals with different sizes are nearly identical with strong PL peaks centered at 451 nm(blue),548 nm,568 nm(yellow),and 616 nm(orange),which indicating varied oxygen vacancies in the structure and induce the formation of new energy levels in the band gap.
Furthermore,the film of the nanocuboids has been fabricated onto various substrates via layer by layer self-assembly technique.The thickness of homogeneous monolayer of In_2O_3 is 6.39-15.15 nm.UV-vis absorption spectroscopy provided evidence for subsequent growth of multilayer film,exhibiting progressive enhancement of optical absorption.PL spectrums of multilayer films were also detected.
3.Fabrication,characterization and photoluminescence properties of In_2O_3 Nanoflowers
A simple solvothermal route based on indium complex as precursor was developed to synthesize 3-dimensional(3D) hierarchical flowerlike nanostructure. Indium oxide with the same flowerlike hierarchical structure was directly obtained in one-step.The In_2O_3 nanoflowers are well dispersed,have a uniform diameter of ca. 30-50 nm nm,and are composed of nanoparticles of ca.3-5 nm size.
Because the decomposition of In(acac)_3was too slow in toluene,the grown speed of In_2O_3 nanocrystals was also too slow.So the random aggregation of produced In_2O_3 nanocrystals was happened to decrease the surface energy rather than grown larger.When increasing reaction time to 24 h,the perfect nanoflowers can be obtained.
The photoluminescence(PL) spectra were used to characterize the products.It is observed that the PL spectrum of In_2O_3 naoflowers at room temperature exhibit peaks centered at 438 nm(blue),546 nm,569 nm(yellow),618 nm(orange) in the range of visible light.
4.Synthesis and photocatalytic property of ultrathinβ-In_2S_3 nanotubes
Ultra thin tetragonalβ-In_2S_3 nanotubes have been successfully synthesized for the first time via a simple solvothermal route.The tubular structure is end-closed,with od ca.10-20 nm,thicknessof tubes wall about 2 nm and lengths more than 1μm.The reaction process was followed the track by XRD,SEM,TEM,FT-IR,HR-TEM,TGA and EA at different times in detail.Furthermore,the effects of reaction parameters on the formation of nanostructures were also discussed,and the formation mechanism was proposed.Lauryl mercaptan decomposed under the solvothermal conditions to release S~(2-),and S~(2-) further reacted with the dissolved In~(3+) in the system to form In_2S_3 species.In_2S_3 nanocrystals were aggragated to form nanosheets.After a rolling process of nanosheets under high temperature or thermal stress,the nanotubes formed.
The optical properties of obtainedβ-In_2S_3 nanotubes were also studied.UV-vis spectrum indicates the strong quantum confinement of the excitonic transition expected forβ-In_2S_3 nanotubes.Furthermore,β-In_2S_3 nanotubes' better photocatalytic property for the degradation of RhB than commercial Degussa P25.
5.Synthesis and characterization of In_2O_3 nanocrystals via hydro/solvothermal routes.
In this chapter,we introduced a kind of convenience route to prepare In_2O_3 nanoparticles and nanobelts.In the hydrothermal/solvothermal system,we use In(NO_3)_3·4H_2O as the indium source,adjusting the hydrolysis reaction of indium salt via control the water content of the system in order to control morphologies of the products.In ethanol solvothermal reaction system,the generated In(OH)_3 from hydrolysis of indium salt further dehydrated to form In_2O_3 nancrystals.The conversion of In(OH)_3 into In_2O_3 can be proposed as a "dissolution-recrystallization" mechanism,and the driving force is the lower solubility of the In_2O_3 compared to the In(OH)_3 in the system.In the hydrothermal system,the indium ions completely hydrolyzed.Due to the alkali of sodium oleate in water can provide plenty of OH~- to promote the growth of nanocrystals,the In(OH)_3 belt-like structure obtained.After heat-treatment at 300℃,In_2O_3 single crystals nanobelts produced.
The as-synthesized In_2O_3 nanocrystals reveal UV absorption around 273,323 nm repectively,exhibiting a distinct blue-shifted to the bulk In_2O_3.Such blue-shift could be contributed to the existence of weak quantum confinement effect.The room temperature PL spectra of as-prepared In_2O_3 nanoparticles and nanobelts are clearly different,which is due to existence of different oxide-deficiency states from the different synthesis routes.
1.溶液法一步合成刚玉型亚稳相三氧化二铟:前驱体对产品物相的影响
利用乙醇溶剂热方法,在较低温度200℃,首次一步直接合成了六方结构的In_2O_3(H-In_2O_3)六边形纳米片。纳米片边长为100-200nm,厚度约为30nm。在甲醇/水存在下,90℃的加热干燥过程中相对较弱键断裂,释放出少量乙酰丙酮配体,即释放出的acac~-,为了平衡电荷,acac~-夺取甲醇分子中的质子形成Hacac分子。生成的甲氧基负离子则占据acac~-让出的空轨道,生成铟离子与甲氧基和乙酰丙酮混和配体配位的配合物。我们通过X射线粉末衍射(XRD)、红外(IR)、热重分析(TGA)、核磁共振(NMR)、X射线光电子能谱(XPS)等技术对此配合物进行了表征,这些表征结果表明配合物分子中存在着少量的甲氧基(-OCH_3)基团。以此配合物为前驱体进行乙醇溶剂热反应,即得到刚玉型亚稳相氧化铟。而乙酰丙酮铟为前驱体的溶剂热反应得到的为立方相的氧化铟(C-In_2O_3)。
为深入理解前驱体的微小差异影响最终产物氧化铟物相的机制,我们通过XRD、IR技术对实验过程进行了跟踪,并对反应上清液进行了~(13)C NMR及~1HNMR分析。结果表明,C-In_2O_3的生成是通过乙酰丙酮铟的简单热分解,而H-In_2O_3则是由于前驱体配合物的水解所得。前驱体间微小的差异导致不同的反应机理进而形成不同物相产物,这在以往的科研工作中经常被忽视。所合成的六方相氧化铟纳米晶与立方相氧化铟以及Degussa P25相比,有着更强的催化降解苯酚的能力。
2.三氧化二铟纳米立方块的合成及其自组装膜
以乙酰丙酮铟为前驱体,在不同的有机溶剂中进行溶剂热反应,得到表面平滑,棱角规则清晰的立方三氧化二铟纳米立方块。反应溶剂由乙醇改变为n-丁醇、n-辛醇、苯,得到的纳米立方块边长从约21nm减小到约12nm、8nm和6nm,厚度从8nm减小到约6nm,5nm和3nm。
在不同溶剂中得到的不同尺寸的氧化铟纳米晶均在可见光区有四个强的发射峰,其中心分别位于451nm(蓝色)、548、568nm(黄色)和616nm(橙色)。这说明样品中含有丰富的氧空位,产生了不同的能级,这样在光激发的过程中使紫外带边发射(NBE)与深能级发射(DL)的比值非常小,因此导致光致发光(PL)光谱上出现四个可见光发射峰。
采用层层自组装技术,将氧化铟无机纳米颗粒自组装成膜。原子力显微镜(AFM)表征表明薄膜表面颗粒分布紧密均匀,单层膜的厚度为6.39-15.15nm。我们利用紫外可见吸收光谱记录了多层膜制备过程,即监测了每次沉积循环后所形成的薄膜的吸收光谱。随着沉积循环次数的增加,薄膜吸收峰的强度近线性增强,这为多层膜组装,厚度逐渐增长提供了证据。同时随沉积循环次数增多,膜的厚度增加,其荧光发光强度呈线性增强。
3.纳米花状In_2O_3级次纳米结构的制备、表征及光学性质
利用乙酰丙酮铟为前驱体,甲苯溶剂热方法制备了具有级次结构的新型花状立方氧化铟,纳米花由粒径为3-5nm的纳米颗粒组成。通过XRD、FT-IR、TEM、HR-TEM等技术对其进行了表征。
由于乙酰丙酮化合物的热分解速度很慢,氧化铟纳米晶生长的速度较慢。在这种情况下,纳米小颗粒之间碰撞聚集的速度要大于纳米晶生长的速度,生成的氧化铟纳米颗粒为了降低其表面能量,开始随意聚集,这样纳米颗粒的聚集体就会渐渐形成。随着反应时间的延长,氧化铟纳米颗粒逐渐聚集形成花状纳米结构。
这种In_2O_3花状纳米结构具有独特的发光性质,发射中心分别处于438nm(蓝)、546nm、569nm(黄)、618nm(橙)处。蓝光和黄色光应归因于光子激发的空穴和占据氧空位的电子的复合。而位于618nm的发射则是由InO_6八面体中的缺陷造成的。
4.硫化铟纳米管的溶剂热合成、表征及其光学性能研究
以硝酸铟In(NO_3)_3·4H_2O作铟源,十二硫醇作硫源,通过吡啶溶剂热反应一步得到β-In_2S_3纳米管。纳米管两端封闭,外径约为10-20nm,管壁厚约2nm,长度达到微米级。HR-TEM照片表明纳米管由β-In_2S_3纳米颗粒无序组装而成。
我们通过TEM、FESEM、XRD、IR、TG、元素分析等手段对在不同时间获得的产品进行了表征,提出了纳米管的形成机制。即In~(3+)在体系中水解首先生成铟的氢氧化物,硫醇在溶剂热条件下分解释放出S~(2-),体系中溶解的In~(3+)与S~(2-)反应并发生异相成核生成硫化铟,同时随反应的进行铟的氢氧化物不断溶解,所形成的硫化铟纳米颗粒聚集成纳米片状结构,纳米片状结构在240℃,一定压力下,发生卷曲形成纳米管。所制备的硫化铟纳米管有着比P25更好的催化降解罗丹明B的能力。
5.氧化铟纳米颗粒及纳米带的合成与表征
在溶剂热体系中,我们利用In(NO_3)_3·4H_2O作为铟源,通过调节体系的含水量来控制铟盐的水解反应,以达到控制产物物相及其形貌的目的。乙醇溶剂热反应体系中,铟盐水解生成In(OH)_3,In(OH)_3然后进一步脱水形成In_2O_3晶粒。In(OH)_3向In_2O_3的相转变可以理解为“溶解-再结晶”机制,而In_2O_3比In(OH)_3具有更低的溶解度则为其驱动力。而在水热体系中,铟离子充分水解,由于油酸钠水溶液适宜的碱度提供了更多的氢氧根离子,促进了In(OH)_3纳米晶的定向生长,得到了纳米带结构的In(OH)_3。进一步在300℃下进行热处理后,即可得到立方相氧化铟单晶纳米带。
UV-vis吸收光谱中,In_2O_3纳米颗粒和纳米带的分别在273,323nm处有强吸收,较块体In_2O_3的UV光谱有大的蓝移,这是弱的量子限域效应所引起的。所合成的氧化铟纳米颗粒及纳米带的室温光致发光光谱有着明显不同,这是由于经过不同的合成路线制备的纳米结构氧化铟具有不同的缺氧状态。
This paper is focused on the controlled synthesis of indium oxide(In_2O_3) and indium sulfide(In_2S_3) nanostructures,n-type semiconducting oxide ofⅢ-Ⅵcompounds,through solution-phase chemistry routes.Investigations are based on three aspects:controlled synthesis,formation mechanisms,and properties and applications.The contents mainly include metastable corundum-type In_2O_3 nanoplates' preparation,the effects of precursors on the products,formation mechanism and photocatalytic properties;the cubic In_2O_3 nanocubes' preparation, size-controlling,the film of the nanocuboids fabricated onto various substrates via layer by layer self-assembly technique and their optical properties;fabrication of Indium oxide with flowerlike hierarchical structure;synthesis of ultra thin tetragonalβ-in_2S_3 nanotubes,formation mechanism,optical and photocatalytic properties; synthesis and characterization of In_2O_3 nanoparticles and nanobelts via hydro/solvothermal routes.Through In_2O_3 and In_2S_3 nanocrystals' preparation, size-controlling,formation mechanisms and optical and photocatalytic properties,we intend to study the intrinsic controlling mechanism of the nanocrystal formation and look for more effective ways to synthesis of nanostructural materials.
1.Direct solution synthesis of corundum-type In_2O_3:effects of precursors on products
Nanostructured metastable corundum-type In_2O_3 was directly synthesized by a low temperature solvothermal method.The as-prepared products were characterized by X-ray diffractions(XRD),Scan Electron Microscopy(SEM),Transmission Electron Microscopy(TEM) and Fourier Transform Infrared(FT-IR) spectrum in detail. H-In_2O_3 nanoparticles exhibit as hexagonal nanoplates with a side length of 100-200 nm and a thickness of ca.30 nm.The effects of precursors on the products were investigated.It is proposed that the existence of-OCH_3 in the H-In_2O_3 precursor leads to a hydrolysis process rather than thermal decomposition to form the H-In_2O_3. Gas-Chromatography(GC) and Nuclear Magnetic Resonance Spectrum(NMR) of reaction solutions also reveal that the formation of the C-In_2O_3 only goes through the simple thermal decomposition of Ln(acac)_3,while the hydrolysis is the main process during the formation of H-In_2O_3.The present direct solution preparation provides a low-temperature route to H-In_2O_3 and there is no crystalline intermediate during the formation of H-In_2O_3.Moreover,the H-In_2O_3 exhibited higher photocatalytic activity for the degradation of phenol than C-In_2O_3 nanocubes and commercial Degussa P25.
2.Synthesis of In_2O_3 nanocuboids and the corresponding self-assembled films
In_2O_3 nanocuboids have been solvothermally synthesized using indium acetylacetonate as precursor.The size of the nanocuboids could be tunable by adjusting the solvent.The particle sizes of the products obtained from ethanol, n-buthanol,n-octanol and benzene are respectively 21,12,8,6 nm.The PL(all the samples excited at 330 nm,room temperature) emission behaviors of the In_2O_3 nanocrystals with different sizes are nearly identical with strong PL peaks centered at 451 nm(blue),548 nm,568 nm(yellow),and 616 nm(orange),which indicating varied oxygen vacancies in the structure and induce the formation of new energy levels in the band gap.
Furthermore,the film of the nanocuboids has been fabricated onto various substrates via layer by layer self-assembly technique.The thickness of homogeneous monolayer of In_2O_3 is 6.39-15.15 nm.UV-vis absorption spectroscopy provided evidence for subsequent growth of multilayer film,exhibiting progressive enhancement of optical absorption.PL spectrums of multilayer films were also detected.
3.Fabrication,characterization and photoluminescence properties of In_2O_3 Nanoflowers
A simple solvothermal route based on indium complex as precursor was developed to synthesize 3-dimensional(3D) hierarchical flowerlike nanostructure. Indium oxide with the same flowerlike hierarchical structure was directly obtained in one-step.The In_2O_3 nanoflowers are well dispersed,have a uniform diameter of ca. 30-50 nm nm,and are composed of nanoparticles of ca.3-5 nm size.
Because the decomposition of In(acac)_3was too slow in toluene,the grown speed of In_2O_3 nanocrystals was also too slow.So the random aggregation of produced In_2O_3 nanocrystals was happened to decrease the surface energy rather than grown larger.When increasing reaction time to 24 h,the perfect nanoflowers can be obtained.
The photoluminescence(PL) spectra were used to characterize the products.It is observed that the PL spectrum of In_2O_3 naoflowers at room temperature exhibit peaks centered at 438 nm(blue),546 nm,569 nm(yellow),618 nm(orange) in the range of visible light.
4.Synthesis and photocatalytic property of ultrathinβ-In_2S_3 nanotubes
Ultra thin tetragonalβ-In_2S_3 nanotubes have been successfully synthesized for the first time via a simple solvothermal route.The tubular structure is end-closed,with od ca.10-20 nm,thicknessof tubes wall about 2 nm and lengths more than 1μm.The reaction process was followed the track by XRD,SEM,TEM,FT-IR,HR-TEM,TGA and EA at different times in detail.Furthermore,the effects of reaction parameters on the formation of nanostructures were also discussed,and the formation mechanism was proposed.Lauryl mercaptan decomposed under the solvothermal conditions to release S~(2-),and S~(2-) further reacted with the dissolved In~(3+) in the system to form In_2S_3 species.In_2S_3 nanocrystals were aggragated to form nanosheets.After a rolling process of nanosheets under high temperature or thermal stress,the nanotubes formed.
The optical properties of obtainedβ-In_2S_3 nanotubes were also studied.UV-vis spectrum indicates the strong quantum confinement of the excitonic transition expected forβ-In_2S_3 nanotubes.Furthermore,β-In_2S_3 nanotubes' better photocatalytic property for the degradation of RhB than commercial Degussa P25.
5.Synthesis and characterization of In_2O_3 nanocrystals via hydro/solvothermal routes.
In this chapter,we introduced a kind of convenience route to prepare In_2O_3 nanoparticles and nanobelts.In the hydrothermal/solvothermal system,we use In(NO_3)_3·4H_2O as the indium source,adjusting the hydrolysis reaction of indium salt via control the water content of the system in order to control morphologies of the products.In ethanol solvothermal reaction system,the generated In(OH)_3 from hydrolysis of indium salt further dehydrated to form In_2O_3 nancrystals.The conversion of In(OH)_3 into In_2O_3 can be proposed as a "dissolution-recrystallization" mechanism,and the driving force is the lower solubility of the In_2O_3 compared to the In(OH)_3 in the system.In the hydrothermal system,the indium ions completely hydrolyzed.Due to the alkali of sodium oleate in water can provide plenty of OH~- to promote the growth of nanocrystals,the In(OH)_3 belt-like structure obtained.After heat-treatment at 300℃,In_2O_3 single crystals nanobelts produced.
The as-synthesized In_2O_3 nanocrystals reveal UV absorption around 273,323 nm repectively,exhibiting a distinct blue-shifted to the bulk In_2O_3.Such blue-shift could be contributed to the existence of weak quantum confinement effect.The room temperature PL spectra of as-prepared In_2O_3 nanoparticles and nanobelts are clearly different,which is due to existence of different oxide-deficiency states from the different synthesis routes.
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