||Synthesis and characteristics of layered tin disulfide nanostructure via hot injection method
||Department of Materials Science and Engineering
為了進一步量測二硫化錫之光電性質，本實驗以旋轉塗佈法將二硫化錫粉末塗佈於光學玻璃上後，經過200 oC的燒結並持溫2小時，使薄膜具有較佳的結晶性以及附著性。由結果可知，二硫化錫單一相所形成的薄膜具有均勻的表面結構以及高度的(001)結晶面，進而影響其光電特性。由吸收光譜的結果可觀察到，二硫化錫薄膜在波長為500奈米之前就有明顯的吸收，且其具有2.35 eV的寬能隙。在電特性上，雖然二硫化錫薄膜具有高達2200 Ω的電阻值，但其在電化學環境下的開路電壓值為0.12 V，遠低於電解水所需的電壓1.23 V，使本材料具有應用於水解製氫催化劑的潛力。
Layered SnS2 nanostructures were synthesized via a facile hot injection method during which the tin precursor was quickly injected into the sulfur precursor and the precipitation of tin and sulfur ions leads to the growth of layered SnS2 nanosheets. In this study, we have altered the precursor concentration and reaction time to analyze the growth mechanism of SnS2. The results show that stable SnS2 nanosheets can be obtained when the precursor ratio of tin and sulfur was 1:5 with a one hour reaction time period and the maximum particle size obtained is about 400 nm. For a prolonged reaction time, the particle size will not increase but only result in a change in the thickness of the layered nanosheets. SnS2 thin films were deposited on a glass substrate using the spin coating technique followed by annealing at 200 oC for 2 hrs. The film structure is uniform and shows a preferred orientation along the (001) plane. Analysis of the UV-visible spectrum shows strong absorption for the SnS2 film in the visible region of the electromagnetic spectrum and its band gap is observed at about 2.4 eV. Furthermore, it can be seen from the I-V curve results that the SnS2 thin film has a resistance of 2200 Ω and its on-set potential is 0.12 V, making it suitable for electrocatalytic applications.
1.1 前言 1
1.2 研究動機 2
2.1 二維奈米材料 3
2.2 二硫化錫之性質及應用 7
2.3 二硫化錫之合成方法 10
2.4 二硫化錫之成長機制 18
3.1 實驗藥品 23
3.2 實驗方法 24
3.2.1 製備二硫化錫粉末 24
3.2.2 製備二硫化錫薄膜 28
3.3 分析儀器 30
3.3.1 X光繞射儀 (X-ray diffraction, XRD) 30
3.3.2 場發射掃描式電子顯微鏡 (Field emission scanning electron microscopy, FE-SEM) 30
3.3.3 高解析穿透式電子顯微鏡 (High resolution transmission electron microscopy, HR-TEM) 31
3.3.4 多功能X光薄膜繞射儀 (Multipurpose X-ray thin film diffraction) 31
3.3.5 紫外光-可見光-近紅外光分光光譜儀 (UV-Visible-NIR spectrophotometer) 32
3.4.6 半導體參數測定儀 (Semiconductor parameter analyzer) 32
3.4.7 恆電位儀 (Potentiostant) 32
3.4.8 熱重分析儀 (Thermal gravim analysis, TGA) 33
4.1 改變硫前驅源濃度對二硫化錫粉末之影響 34
4.2 改變反應時間對二硫化錫粉末之影響 41
4.3 二硫化錫之成長機制 47
4.4 二硫化錫薄膜之物理性質 51
4.5 二硫化錫薄膜之光電特性 56
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