ZnSe纳米材料的制备及光学、光催化性能研究
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摘要
ZnSe是一种非常重要的宽禁带Ⅱ—Ⅵ族半导体材料，在可见光范围内具有优异的光电催化及光电转化活性，可以用于制作蓝色发光器件，红外热成像仪，全天候光学装置及太阳能电池，在通信，复印，高密度的信息存储，高分辨率的图像显示，信号指示以及生物医学和基础研究等方面的应用前景非常广阔。虽然有大量的研究工作者致力于光催化研究领域，但是关于ZnSe半导体材料在光催化领域的应用研究还不是很完善。ZnSe半导体材料常用的制备方法主要有化学气相沉积法、电沉积法、溶胶凝胶法、共沉淀法和分子束外延生长法等。其中，水热/溶剂热法因其制备工艺简单、投资少、污染小等优点而成为一种制备ZnSe纳米材料的常用方法。
本论文中采用溶剂热法成功地合成了硒化锌量子点、纳米片和纳米颗粒。利用X射线衍射仪、透射电镜、能谱分析仪、紫外显微拉曼-荧光光谱仪、紫外可见分光光度计等测试手段对样品的结构、形貌、以及光学、光催化性能进行详细的研究。主要内容如下：
（1）利用溶剂热法制备六角纤锌矿结构的硒化锌量子点和立方闪锌矿结构的硒化锌纳米颗粒，其中，硒化锌量子点的尺寸仅为3.5nm，同时硒化锌纳米颗粒的尺寸约为21nm。对比研究了两种不同结构样品的生长机制。硒化锌量子点的光致发光谱显示出样品在422nm处存在强的近带边发射峰，与体材料ZnSe相比，发生明显蓝移，这主要是由量子限域效应引起的。然而，闪锌矿结构的硒化锌纳米颗粒的近带边发射峰处于472nm。研究了六角纤锌矿结构的硒化锌量子点和立方闪锌矿结构的硒化锌纳米颗粒的拉曼衍射峰，拉曼谱显示两种不同结构样品的拉曼峰与体材料相比都向低频方向移动，同时，ZnSe量子点的拉曼峰发生了一定的宽化，这是由于量子点的小尺寸引起的。
（2）利用溶剂热法通过调节乙二胺与水的体积比合成不同形貌的硒化锌纳米材料。当乙二胺与水的体积比从1：1增加到5：1时，样品的形貌从各向同性的纳米颗粒变为高度各向异性的纳米片。XRD结果显示无论是硒化锌纳米颗粒还是硒化锌纳米片，其结构都是亚稳的六角纤锌矿结构。TEM结果显示，纳米颗粒是均匀球形，并且尺寸大约是7nm；而大尺寸的纳米片长度达到4μm，宽度达到3μm，并且具有单晶特性。通过对纳米片的生长机制进行研究，发现硒化锌纳米片是由纳米颗粒沿同一方向平行排列组成的，这是因为乙二胺作为溶剂具有模板的作用。纳米片和纳米颗粒的光致发光谱显示样品都在422nm处出现近带边发射峰，与体材料相比发生了明显蓝移。在紫外灯照射下对罗丹明B溶液的降解过程说明纳米颗粒和纳米片都具有光催化活性，对比之后得出纳米片的光催化效率更高。
（3）利用不同溶剂制备出立方闪锌矿结构的硒化锌纳米粒子，首先利用EDTA作为溶剂制备出不同尺寸的硒化锌纳米粒子，详细研究了反应时间对ZnSe纳米材料尺寸和光学性质的影响。随着纳米颗粒的尺寸从21nm降至7nm，室温下样品的光致发光谱显示出样品的近带边发射峰发生了7nm的红移，缺陷相关的发射带变宽且强度更强。再分别利用乙二醇、三乙醇胺作为溶剂，制备出ZnSe纳米材料，研究了不同溶剂条件下制备得到的ZnSe纳米材料的光学和光催化性能。对比光催化研究结果表明，以三乙醇胺为溶剂制备的硒化锌，其光催化效率大幅度提高，并研究了影响硒化锌光催化效率的因素。
ZnSe is an important semiconductor material (AII-BVI group) with widedirect band gap (2.67eV) at room temperature and large exciton binding energy(21meV). ZnSe has attracted much more attention recently due to their greatpotential for fundamental research and practical applications. The ZnSenanomaterials have the wide-ranging optoelectronic applications including bluelight-emitting diodes, photodetectors, room-temperature excitonic devices,full-color displays. Furthermore, due to their low toxicity (without heavy metalions), ZnSe nanomaterials are potential blue fluorescent biological labels.Although attempts have been tried, the photodegradation in presence of ZnSenanomaterials has seldom been reported. ZnSe nanomaterials have beensuccessfully synthesized via various methods, such as CVD, electrodepositionmethod, sol-gel, coprecipitation method, MBE. The solvothermal method hasbeen most widely used because it requires a relatively low temperature, cheapprecursors of low toxicity, which is simple and easy to operate.
In this paper, the ZnSe quantum dots, nanosheets and nanoparticles wereobtained by a solvothermal method. The structure, morphologies, opticalproperties and photocatalytic activity have been investigated in detail by themethods of X-ray Diffraction (XRD), transmission electron microscope (TEM),energy dispersive x-ray analysis (EDAX), UV Raman and fluorescencespectrometer and UV-Vis. The major achievement obtained is as follow:
(1) ZnSe quantum dots and nanoparticles were obtained by annealing the precursors which were prepared by a solvothermal method. The ZnSequantum dots were about3.5nm, while the ZnSe nanoparticles wereabout21nm, as observed using TEM. The growth mechanisms for thetwo samples with different structures were discussed. The ZnSe quantumdots with the wurtzite structure exhibited a strong near band-edgeemission (NBE) peak centered at422nm which was blue-shifted incomparison with that of the bulk ZnSe, which mainly caused by thequantum confinement effect. However, the zinc blende ZnSenanoparticles exhibited near-band-edge luminescence peak centered at472nm. The Raman spectrum of the ZnSe quantum dots with wurtzitestructure and nanoparticles with cubic structure were studied. The LO andTO phonon peaks of the ZnSe quantum dots and nanoparticles wereshifted towards the lower frequency. Large broadening of Raman spectrawere observed in the ZnSe quantum dots.
(2) ZnSe nanocrystals with different morpholygies were obtained byannealing the precursors prepared via a solvothermal process withdifferent volume ratio of ethylenediamine and water. When the volumeratio increased from1:1to5:1, the morphologies changed from theisotropic nanoparticles to the highly anisotropic nanosheets. The X-raydiffraction (XRD) results showed both the ZnSe nanoparticles andnanosheets were metastable wurtzite crystal phase. The results of TEMfound that the nanoparticles were uniform and the average size was about7nm, while the large-scale nanosheets with length up to4μm and widthup to3μm had the single crystalline nature. By investigating the growthmechanism of the ZnSe nanosheets, the nanocrystal unit was assembledin a parallel orientation into the sheet morphology due to the solventcoordination molecular template effect of the EN. The nanoparticles andnanosheets exhibited the NBE peak centered at422nm, which wasblue-shifted compared with the PL spectra of bulk WZ ZnSe. Theinvestigation of the photocatalytic activity for the ZnSe nanoparticles andnanosheets showed that the nanosheets were more suitable for thedegradation of Rhodamine B under UV radiation.
(3) ZnSe nanoparticles with cubic structure were obtained by using differentsolvents. ZnSe nanoparticles with different sizes were successfully prepared using EDTA by a hydrothermal method. The effect of reactiontime on the sizes and optical properties of ZnSe nanoparticles wereinvestigated. The position of near-band-edge emission peak in theroom-temperature PL spectra showed a red-shift ranging from472nm to479nm with particle size decreasing from21nm to7nm, while the lowdefect-related emission band became broader and stronger. Using theethanediol or triethanolamine as the solvent, the optical properties and thephotocatalytic activity of the ZnSe nanomaterials obtained by usingdifferent solvents were studied. The investigation of the photocatalyticactivity showed that the ZnSe obtained by using triethanolamine had highphotocatalytic activity. The factors which influenced the photocatalyticactivities of ZnSe nanomaterials were studied.
本论文中采用溶剂热法成功地合成了硒化锌量子点、纳米片和纳米颗粒。利用X射线衍射仪、透射电镜、能谱分析仪、紫外显微拉曼-荧光光谱仪、紫外可见分光光度计等测试手段对样品的结构、形貌、以及光学、光催化性能进行详细的研究。主要内容如下：
（1）利用溶剂热法制备六角纤锌矿结构的硒化锌量子点和立方闪锌矿结构的硒化锌纳米颗粒，其中，硒化锌量子点的尺寸仅为3.5nm，同时硒化锌纳米颗粒的尺寸约为21nm。对比研究了两种不同结构样品的生长机制。硒化锌量子点的光致发光谱显示出样品在422nm处存在强的近带边发射峰，与体材料ZnSe相比，发生明显蓝移，这主要是由量子限域效应引起的。然而，闪锌矿结构的硒化锌纳米颗粒的近带边发射峰处于472nm。研究了六角纤锌矿结构的硒化锌量子点和立方闪锌矿结构的硒化锌纳米颗粒的拉曼衍射峰，拉曼谱显示两种不同结构样品的拉曼峰与体材料相比都向低频方向移动，同时，ZnSe量子点的拉曼峰发生了一定的宽化，这是由于量子点的小尺寸引起的。
（2）利用溶剂热法通过调节乙二胺与水的体积比合成不同形貌的硒化锌纳米材料。当乙二胺与水的体积比从1：1增加到5：1时，样品的形貌从各向同性的纳米颗粒变为高度各向异性的纳米片。XRD结果显示无论是硒化锌纳米颗粒还是硒化锌纳米片，其结构都是亚稳的六角纤锌矿结构。TEM结果显示，纳米颗粒是均匀球形，并且尺寸大约是7nm；而大尺寸的纳米片长度达到4μm，宽度达到3μm，并且具有单晶特性。通过对纳米片的生长机制进行研究，发现硒化锌纳米片是由纳米颗粒沿同一方向平行排列组成的，这是因为乙二胺作为溶剂具有模板的作用。纳米片和纳米颗粒的光致发光谱显示样品都在422nm处出现近带边发射峰，与体材料相比发生了明显蓝移。在紫外灯照射下对罗丹明B溶液的降解过程说明纳米颗粒和纳米片都具有光催化活性，对比之后得出纳米片的光催化效率更高。
（3）利用不同溶剂制备出立方闪锌矿结构的硒化锌纳米粒子，首先利用EDTA作为溶剂制备出不同尺寸的硒化锌纳米粒子，详细研究了反应时间对ZnSe纳米材料尺寸和光学性质的影响。随着纳米颗粒的尺寸从21nm降至7nm，室温下样品的光致发光谱显示出样品的近带边发射峰发生了7nm的红移，缺陷相关的发射带变宽且强度更强。再分别利用乙二醇、三乙醇胺作为溶剂，制备出ZnSe纳米材料，研究了不同溶剂条件下制备得到的ZnSe纳米材料的光学和光催化性能。对比光催化研究结果表明，以三乙醇胺为溶剂制备的硒化锌，其光催化效率大幅度提高，并研究了影响硒化锌光催化效率的因素。
ZnSe is an important semiconductor material (AII-BVI group) with widedirect band gap (2.67eV) at room temperature and large exciton binding energy(21meV). ZnSe has attracted much more attention recently due to their greatpotential for fundamental research and practical applications. The ZnSenanomaterials have the wide-ranging optoelectronic applications including bluelight-emitting diodes, photodetectors, room-temperature excitonic devices,full-color displays. Furthermore, due to their low toxicity (without heavy metalions), ZnSe nanomaterials are potential blue fluorescent biological labels.Although attempts have been tried, the photodegradation in presence of ZnSenanomaterials has seldom been reported. ZnSe nanomaterials have beensuccessfully synthesized via various methods, such as CVD, electrodepositionmethod, sol-gel, coprecipitation method, MBE. The solvothermal method hasbeen most widely used because it requires a relatively low temperature, cheapprecursors of low toxicity, which is simple and easy to operate.
In this paper, the ZnSe quantum dots, nanosheets and nanoparticles wereobtained by a solvothermal method. The structure, morphologies, opticalproperties and photocatalytic activity have been investigated in detail by themethods of X-ray Diffraction (XRD), transmission electron microscope (TEM),energy dispersive x-ray analysis (EDAX), UV Raman and fluorescencespectrometer and UV-Vis. The major achievement obtained is as follow:
(1) ZnSe quantum dots and nanoparticles were obtained by annealing the precursors which were prepared by a solvothermal method. The ZnSequantum dots were about3.5nm, while the ZnSe nanoparticles wereabout21nm, as observed using TEM. The growth mechanisms for thetwo samples with different structures were discussed. The ZnSe quantumdots with the wurtzite structure exhibited a strong near band-edgeemission (NBE) peak centered at422nm which was blue-shifted incomparison with that of the bulk ZnSe, which mainly caused by thequantum confinement effect. However, the zinc blende ZnSenanoparticles exhibited near-band-edge luminescence peak centered at472nm. The Raman spectrum of the ZnSe quantum dots with wurtzitestructure and nanoparticles with cubic structure were studied. The LO andTO phonon peaks of the ZnSe quantum dots and nanoparticles wereshifted towards the lower frequency. Large broadening of Raman spectrawere observed in the ZnSe quantum dots.
(2) ZnSe nanocrystals with different morpholygies were obtained byannealing the precursors prepared via a solvothermal process withdifferent volume ratio of ethylenediamine and water. When the volumeratio increased from1:1to5:1, the morphologies changed from theisotropic nanoparticles to the highly anisotropic nanosheets. The X-raydiffraction (XRD) results showed both the ZnSe nanoparticles andnanosheets were metastable wurtzite crystal phase. The results of TEMfound that the nanoparticles were uniform and the average size was about7nm, while the large-scale nanosheets with length up to4μm and widthup to3μm had the single crystalline nature. By investigating the growthmechanism of the ZnSe nanosheets, the nanocrystal unit was assembledin a parallel orientation into the sheet morphology due to the solventcoordination molecular template effect of the EN. The nanoparticles andnanosheets exhibited the NBE peak centered at422nm, which wasblue-shifted compared with the PL spectra of bulk WZ ZnSe. Theinvestigation of the photocatalytic activity for the ZnSe nanoparticles andnanosheets showed that the nanosheets were more suitable for thedegradation of Rhodamine B under UV radiation.
(3) ZnSe nanoparticles with cubic structure were obtained by using differentsolvents. ZnSe nanoparticles with different sizes were successfully prepared using EDTA by a hydrothermal method. The effect of reactiontime on the sizes and optical properties of ZnSe nanoparticles wereinvestigated. The position of near-band-edge emission peak in theroom-temperature PL spectra showed a red-shift ranging from472nm to479nm with particle size decreasing from21nm to7nm, while the lowdefect-related emission band became broader and stronger. Using theethanediol or triethanolamine as the solvent, the optical properties and thephotocatalytic activity of the ZnSe nanomaterials obtained by usingdifferent solvents were studied. The investigation of the photocatalyticactivity showed that the ZnSe obtained by using triethanolamine had highphotocatalytic activity. The factors which influenced the photocatalyticactivities of ZnSe nanomaterials were studied.
引文
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