水熱法制備硫化鎘納米材料及其表征
本文關(guān)鍵詞: 水熱法 硫化鎘 形貌 晶體結(jié)構(gòu) 光學性質(zhì) 出處:《蘭州理工大學》2011年碩士論文 論文類型:學位論文
【摘要】:半導體納米材料由于具有許多優(yōu)異的性質(zhì),從而引起人們極大的研究興趣。其中的硫化鎘半導體材料在光、電、磁、催化等方面具有應用潛能,發(fā)展前景廣闊,已引起了人們的高度重視。因此本文將就利用水熱法制備的硫化鎘納米顆粒和納米棒進行報道。 首先,利用水熱法成功地制備了硫化鎘納米顆粒,并利用X射線衍射(XRD)、透射電子顯微鏡(TEM)和相應選區(qū)電子衍射(SAED)等測試手段對樣品的晶體結(jié)構(gòu)、形貌和粒度等特征進行了表征分析。實驗結(jié)果表明:適當控制某些工藝參數(shù)可以改變硫化鎘納米晶的晶型。在一定溫度下,硫化鎘可以從低溫穩(wěn)定態(tài),即立方晶相,向高溫穩(wěn)定態(tài),即六角晶相轉(zhuǎn)化;改變反應時間,硫化鎘也可以從立方晶相向六角晶相轉(zhuǎn)化,延長反應時間樣品的結(jié)晶效果更好。 其次,改變試驗條件用水熱法成功制備了硫化鎘納米棒,利用X射線衍射(XRD)、透射電子顯微鏡(TEM)和高分辨透射電子顯微鏡(HRTEM)對樣品的晶體結(jié)構(gòu)、形貌進行性能表征。實驗結(jié)果表明,該法制備的硫化鎘納米棒為纖鋅礦結(jié)構(gòu),直徑為48~74 nm,沿[001]方向擇優(yōu)生長。同時,以自制的硫化鎘為光催化劑,鎢燈模擬可見光,研究了硫化鎘對活性染料亞甲基藍的的光催化降解過程?疾炝斯庹諘r間、催化劑用量、污染物的初始濃度對光催化過程的影響。也對硫化鎘納米晶的形成機理進行了初步的探討。 同時,采用紫外-可見和熒光分光光度計表征了樣品的光學性質(zhì),結(jié)果發(fā)現(xiàn):納米級的硫化鎘,無論是顆粒還是棒狀的,吸收峰相對塊體材料都發(fā)生了藍移,但是隨著反應溫度的升高,吸收峰會產(chǎn)生一定的紅移。由于表面缺陷的影響,發(fā)光峰也發(fā)生了大幅度的紅移。 另外,利用陽極弧放電等離子體技術(shù)成功地制備了銅納米顆粒,并利用X射線衍射(XRD)、透射電子顯微鏡(TEM)和相應選區(qū)電子衍射(SAED)、BET氮吸附等測試手段對樣品的晶體結(jié)構(gòu)、形貌、比表面積和粒度等特征進行了表征分析,并計算了其不同晶面的晶格參數(shù)。實驗結(jié)果表明:銅納米顆粒為fcc晶態(tài)結(jié)構(gòu),晶格畸變表現(xiàn)為晶格收縮。
[Abstract]:Semiconductor nanomaterials have attracted great interest because of their excellent properties. Among them, cadmium sulfide semiconductor materials have the potential to be applied in light, electricity, magnetism, catalysis and so on. Therefore, cadmium sulfide nanoparticles and nanorods prepared by hydrothermal method are reported in this paper. Firstly, cadmium sulfide nanoparticles were successfully prepared by hydrothermal method. The crystal structures of the samples were measured by X-ray diffraction (XRD), transmission electron microscopy (TEM) and corresponding selected area electron diffraction (SAE). The morphology and particle size of the nanocrystalline were characterized and analyzed. The experimental results show that the crystal form of cadmium sulfide nanocrystalline can be changed by controlling some technological parameters properly. At a certain temperature, cadmium sulfide can be stabilized from the low temperature state, that is, cubic crystal phase. When the reaction time is changed, cadmium sulfide can also be transformed from cubic phase to hexagonal phase, and the crystallization effect of the sample can be improved by prolonging the reaction time. Secondly, cadmium sulfide nanorods were successfully prepared by hydrothermal method under different experimental conditions. The crystal structures of the samples were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and high resolution transmission electron microscope (HRTEM). The morphology of the nanorods was characterized. The experimental results showed that the nanorods prepared by this method were wurtzite structure with a diameter of 480.74 nm and preferred growth along the direction of [001]. At the same time, using the self-made cadmium sulfide as the photocatalyst, the tungsten lamp was used to simulate the visible light. The photocatalytic degradation of reactive dye methylene blue by cadmium sulfide was studied. The effect of the initial concentration of pollutants on the photocatalytic process and the formation mechanism of cadmium sulfide nanocrystals were also discussed. At the same time, the optical properties of the samples were characterized by UV-Vis and fluorescence spectrophotometer. The results showed that the absorption peaks of nano-scale cadmium sulfide, whether granular or rod-like, had a blue shift in relation to bulk materials. However, with the increase of the reaction temperature, the absorption summit produces a certain red shift. Due to the influence of surface defects, the luminescence peak also has a large red shift. In addition, copper nanoparticles were successfully prepared by anodic arc discharge plasma technique. The crystal structure and morphology of the samples were measured by X-ray diffraction (XRDX), transmission electron microscopy (TEM) and nitrogen adsorption of the corresponding selected area electron diffraction (SAEDET). The characteristics of specific surface area and particle size were analyzed and the lattice parameters of different crystal planes were calculated. The experimental results show that copper nanoparticles are fcc crystal structure and lattice distortion is lattice shrinkage.
【學位授予單位】:蘭州理工大學
【學位級別】:碩士
【學位授予年份】:2011
【分類號】:TB383.1
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