有机分子辅助的半导体纳米材料的控制合成与性能研究
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摘要
本论文进一步丰富和发展了水热／溶剂热技术在合成半导体纳米材料上的应用,利用有机分子辅助控制合成几种典型的半导体纳米材料,通过调节合成条件来控制产物的形貌,对合成的产物进行性能测试,期望所制备出的材料具有特殊的物理和化学性质。本论文的具体内容归纳如下：
1.通过酒石酸和L-半胱氨酸共同作用,在水相中于180℃水热制备了非晶的蜂窝状Sb2S3微球,直径大约为3μm。FTIR、EDS、XPS分析结果均证实非晶态微球的成分是Sb2S3。在管式炉中250℃热处理得到正交相晶体Sb2S3 (JCPDS 06-0474),晶格常数为a=11.22A,b=11.31A,c=3.839A,煅烧后的产物保持了蜂窝状的形貌。实验结果分析表明酒石酸和L-半胱氨酸对形成非晶的蜂窝状Sb2S3微球起到至关重要的作用。此外,蜂窝状Sb2S3微球的形成机理可以用晶体生长的聚集机理来解释。相关工作发表在European Journal of Inorganic Chemistry上。
2.利用L-赖氨酸的辅助作用,在水相中于200℃合成了纳米片组装的三维(3 D)的锡酸锌(Zn2Sn04)空心八面体分级结构。相比于其他需要高温热处理获得三维(3D) Zn2Sn04材料,本章采用的方法具有一定的优越性,并通过调节反应温度、氢氧化钠和L-赖氨酸的添加量实现对产物形貌和物相的控制。在对反应时间影响产物的研究基础上,探讨了纳米片组装的三维(3D) Zn2SnO4空心八面体分级结构的形成机理。结果表明氢氧化钠和L-赖氨酸的添加量对空心八面体形状的形成起到了决定性的作用。产物的室温光致发光谱图说明所制备的产物在500～600 nm有很强的发光性能。该项工作发表在Chinese Journal of Inorganic Chemistry上。
3.利用硫代乙醇酸(TGA)的配位作用并作为反应原料,在180℃中水热处理合成了纳米颗粒附着的一维棒状有机／无机复合结构,棒的直径100～500nm,纳米颗粒的尺寸为50 nm左右。多种分析手段证实纳米颗粒为纤锌矿CdS,棒为Cd2+和TGA配合物,结果确定此复合物的组分为CdS0.65/Cd-TGA0.35。在400℃下于管式炉中热处理获得相应的纯相CdS超结构材料,并且保持了前驱物的形貌。光致发光谱(PL)结果表明退火前后产物都显示两个不同的发光位置：一个是480 nm的绿色发射带,另一个是570 nm可见光发射带,但有机／无机复合物的发光强度比退火后产物(纯相的CdS)的发光强度高很多。此外,在油酸分子的作用下,于乙醇胺和水的混合溶剂中制备了子弹头状的六方相CdS纳米粒子(JCPDS No.80-0006)晶格常数a=4.142 A, c=6.724 A,长约为100～150 nm、宽为80～120 nm。最后利用先前制备的有机／无机复合物作为自牺牲模板,在与分别含有Se2-和Te2-的水溶液中室温搅拌反应制备了直径在150～400 nm之间的CdSe和CdTe纳米管。
The goal of this dissertation is to enrich and develop hydro-/solvothermal route. Several representative semiconductor functional materials were successfully controllable synthesized by organic molecule assistance. The morphologies of the products were realized by adjusting the reaction conditions. And the formation mechanism and optical properties of products are also discussed. It is expected that the as-obtained products possess some novel physical and chemical properties. The details are summarized as follows:
1. Alveolate amorphous Sb2S3 microspheres about 3μm in diameter were hydrothermally synthesized in aqueous solution without surfactant at 180℃using SbCl3, L-cysteine and tartaric acid as starting materials. After annealed at 250℃for 3 h in nitrogen atmosphere, polycrystalline Sb2S3 hollow spheres were obtained. Results show that tartaric acid and L-cysteine play a key role in the formation of such hierarchical structures. In addition, the possible aggregation mechanism was proposed to illustrate the formation of Sb2S3 microspheres based on the experimental results and analyses. The above results of research have been published in European Journal of Inorganic Chemistry.
2. Hollow octahedral Zn2SnO4 (ZTO) hierarchical structures were hydrothermally synthesized starting from Zn(Ac)2, SnCl4 and L-lysine in NaOH solution at 200℃. The XRD result indicates a face-centered cubic phase for the as-prepared octahedral ZTO product with lattice constant a of 0.8650 nm. Results also demonstrate that the adding amount of NaOH and L-lysine has an immense function in the morphology control of octahedral ZTO hierarchical structures. The photoluminescences of the as-fabricated ZTO products with different shapes all display a broad strong green emission band at 500～600 nm but different in intensity at room temperature. The above results of research have been published in Chinese Journal of Inorganic Chemistry.
3. Cadmium sulfide rod-bundle structures decorated with nanoparticles have been synthesized via calcinations of inorganic/ organic composite precursor. The precursor was hydrothermally synthesized at 180℃using thioglycolic acid (TGA) and cadmium acetate as starting materials. The composition and phase structure of the precursor were investigated in detail. After detailed analyses, the precursor could be defined as CdS0.65/Cd-TGAo.35 and further completely transformed to wurtzite CdS through a thermal decomposition process at 400℃in air. The photoluminescence (PL) intensity of precursor is about hundred times than that of wurtzite CdS while with the same PL position. And when using ethanolamine and water as mixed solvent, wurtzite CdS nanocrystals with bullet-like morphology were synthesized by oleic acid assisted. Finally, cadmium chalcogenide (CdE, E= Se, Te) polycrystalline nanotubes were realized from the precursor at room temperature. The transformation from the precusor to CdSe and CdTe nanotubes were performed under constant stirring at room temperature in aqueous solution containing S2-, Se2- and Te2-, respectively. The nanotube diameter can be controlled from 150 to 400 nm related to the dimension of precursor.
1.通过酒石酸和L-半胱氨酸共同作用,在水相中于180℃水热制备了非晶的蜂窝状Sb2S3微球,直径大约为3μm。FTIR、EDS、XPS分析结果均证实非晶态微球的成分是Sb2S3。在管式炉中250℃热处理得到正交相晶体Sb2S3 (JCPDS 06-0474),晶格常数为a=11.22A,b=11.31A,c=3.839A,煅烧后的产物保持了蜂窝状的形貌。实验结果分析表明酒石酸和L-半胱氨酸对形成非晶的蜂窝状Sb2S3微球起到至关重要的作用。此外,蜂窝状Sb2S3微球的形成机理可以用晶体生长的聚集机理来解释。相关工作发表在European Journal of Inorganic Chemistry上。
2.利用L-赖氨酸的辅助作用,在水相中于200℃合成了纳米片组装的三维(3 D)的锡酸锌(Zn2Sn04)空心八面体分级结构。相比于其他需要高温热处理获得三维(3D) Zn2Sn04材料,本章采用的方法具有一定的优越性,并通过调节反应温度、氢氧化钠和L-赖氨酸的添加量实现对产物形貌和物相的控制。在对反应时间影响产物的研究基础上,探讨了纳米片组装的三维(3D) Zn2SnO4空心八面体分级结构的形成机理。结果表明氢氧化钠和L-赖氨酸的添加量对空心八面体形状的形成起到了决定性的作用。产物的室温光致发光谱图说明所制备的产物在500～600 nm有很强的发光性能。该项工作发表在Chinese Journal of Inorganic Chemistry上。
3.利用硫代乙醇酸(TGA)的配位作用并作为反应原料,在180℃中水热处理合成了纳米颗粒附着的一维棒状有机／无机复合结构,棒的直径100～500nm,纳米颗粒的尺寸为50 nm左右。多种分析手段证实纳米颗粒为纤锌矿CdS,棒为Cd2+和TGA配合物,结果确定此复合物的组分为CdS0.65/Cd-TGA0.35。在400℃下于管式炉中热处理获得相应的纯相CdS超结构材料,并且保持了前驱物的形貌。光致发光谱(PL)结果表明退火前后产物都显示两个不同的发光位置：一个是480 nm的绿色发射带,另一个是570 nm可见光发射带,但有机／无机复合物的发光强度比退火后产物(纯相的CdS)的发光强度高很多。此外,在油酸分子的作用下,于乙醇胺和水的混合溶剂中制备了子弹头状的六方相CdS纳米粒子(JCPDS No.80-0006)晶格常数a=4.142 A, c=6.724 A,长约为100～150 nm、宽为80～120 nm。最后利用先前制备的有机／无机复合物作为自牺牲模板,在与分别含有Se2-和Te2-的水溶液中室温搅拌反应制备了直径在150～400 nm之间的CdSe和CdTe纳米管。
The goal of this dissertation is to enrich and develop hydro-/solvothermal route. Several representative semiconductor functional materials were successfully controllable synthesized by organic molecule assistance. The morphologies of the products were realized by adjusting the reaction conditions. And the formation mechanism and optical properties of products are also discussed. It is expected that the as-obtained products possess some novel physical and chemical properties. The details are summarized as follows:
1. Alveolate amorphous Sb2S3 microspheres about 3μm in diameter were hydrothermally synthesized in aqueous solution without surfactant at 180℃using SbCl3, L-cysteine and tartaric acid as starting materials. After annealed at 250℃for 3 h in nitrogen atmosphere, polycrystalline Sb2S3 hollow spheres were obtained. Results show that tartaric acid and L-cysteine play a key role in the formation of such hierarchical structures. In addition, the possible aggregation mechanism was proposed to illustrate the formation of Sb2S3 microspheres based on the experimental results and analyses. The above results of research have been published in European Journal of Inorganic Chemistry.
2. Hollow octahedral Zn2SnO4 (ZTO) hierarchical structures were hydrothermally synthesized starting from Zn(Ac)2, SnCl4 and L-lysine in NaOH solution at 200℃. The XRD result indicates a face-centered cubic phase for the as-prepared octahedral ZTO product with lattice constant a of 0.8650 nm. Results also demonstrate that the adding amount of NaOH and L-lysine has an immense function in the morphology control of octahedral ZTO hierarchical structures. The photoluminescences of the as-fabricated ZTO products with different shapes all display a broad strong green emission band at 500～600 nm but different in intensity at room temperature. The above results of research have been published in Chinese Journal of Inorganic Chemistry.
3. Cadmium sulfide rod-bundle structures decorated with nanoparticles have been synthesized via calcinations of inorganic/ organic composite precursor. The precursor was hydrothermally synthesized at 180℃using thioglycolic acid (TGA) and cadmium acetate as starting materials. The composition and phase structure of the precursor were investigated in detail. After detailed analyses, the precursor could be defined as CdS0.65/Cd-TGAo.35 and further completely transformed to wurtzite CdS through a thermal decomposition process at 400℃in air. The photoluminescence (PL) intensity of precursor is about hundred times than that of wurtzite CdS while with the same PL position. And when using ethanolamine and water as mixed solvent, wurtzite CdS nanocrystals with bullet-like morphology were synthesized by oleic acid assisted. Finally, cadmium chalcogenide (CdE, E= Se, Te) polycrystalline nanotubes were realized from the precursor at room temperature. The transformation from the precusor to CdSe and CdTe nanotubes were performed under constant stirring at room temperature in aqueous solution containing S2-, Se2- and Te2-, respectively. The nanotube diameter can be controlled from 150 to 400 nm related to the dimension of precursor.
引文
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