合成錳摻雜硒化鎘團簇物負載碳材的鑑定
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2023
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本研究第一部份透過元素硒粉末代替價格昂貴的硒脲作為改良硒前驅物合成魔術尺寸硒化鎘奈米團簇物((CdSe)13 MSCs)，透過紫外光-可見光譜儀、X光粉末繞射、感應耦合電漿放射光譜、元素分析、紅外光譜、固態核磁共振光譜、DFT理論計算等，證實其同樣為(CdSe)13 MSCs，亦發現與原方法不同地方，替換前驅物後，表面配體由單純胺基組成胺基與醋酸根共配位，並由DFT計算出較大的放熱焓輔佐確認醋酸根增強了反應穩定性。之後皆引入具有未成對電子的二價錳離子以提供比對，透過X光粉末繞射、紫外光-可見光光譜、螢光光譜、感應耦合電漿放射光譜、X光吸收光譜延伸精細結構，得知硒粉合成具較高的錳有效摻雜(最高有效摻雜濃度可達13.5%)、放光強度。第二部份將錳摻雜(CdSe)13 MSCs之光學性質進行延伸，之後測量反射式光致發光光譜並在反覆填滿/阻隔大氣下測量放光性質之差異，揭示氧氣對錳放光進行暫時性干擾而下降，再除去氧氣後會上升，形成可逆的螢光猝滅趨勢，以探討磷光性質半導體對氣體傳感之應用可能。第三部份以氧化石墨烯作為生長模板，一來限制(CdSe)13 MSC均勻生長，二來使錳離子能夠有效分散，以X光粉末繞射、紫外光-可見光光譜得知透過螢光光譜、磷光半生期光譜、電子順磁共振光譜儀、電化學儀鑑定，得知將錳離子之光生載流子轉移至GO以抑制電子電洞複合(PL-lifetime、EIS)降低阻抗，導致螢光猝滅並且產生強電流響應，期望尋找半導體複合材料之應用可能性。
In the first part of this study, the magic size cadmium selenide nanoclusters ((CdSe)13 MSCs) were synthesized by replacing the expensive selenourea with elemental selenium powder as an improved selenium precursor. Through ultraviolet-visible spectroscopy, X-ray powder diffraction, inductively coupled plasma emission spectroscopy, elemental analysis, infrared spectroscopy, solid-state nuclear magnetic resonance spectroscopy, DFT theoretical calculations, etc., it was confirmed that they were also (CdSe) 13 MSCs. Reaction stability and increased crystallinity. Afterwards, divalent manganese ions with unpaired electrons were introduced to provide comparison. Through X-ray powder diffraction, ultraviolet-visible light spectroscopy, fluorescence spectroscopy, inductively coupled plasma emission spectroscopy, and X-ray absorption spectroscopy to extend the fine structure, it is known that the synthesis of selenium powder has higher manganese effective doping and emission intensity.The second part extends the optical properties of manganese-doped (CdSe)13 MSCs, and then measures the reflective photoluminescence spectrum and the difference in light emission properties under repeated filling/blocking atmospheres, revealing that oxygen temporarily interferes with manganese light emission and then decreases, and then rises after removing oxygen, forming a reversible fluorescence quenching trend, in order to explore the possible application of phosphorescent semiconductors to gas sensing.The third part uses graphene oxide as a growth template to limit the uniform growth of (CdSe)13 MSC, and to enable effective dispersion of manganese ions. X-ray powder diffraction and ultraviolet-visible light spectroscopy are used to identify through fluorescence spectroscopy, phosphorescence half-lifetime spectroscopy, electron paramagnetic resonance spectroscopy, and electrochemical instrument identification. It is known that the photogenerated carriers of manganese ions are transferred to GO to inhibit electron-hole recombination, resulting in fluorescence quenching and possible photoresponse. It is expected to find the application possibility of semiconductor composite materials.
In the first part of this study, the magic size cadmium selenide nanoclusters ((CdSe)13 MSCs) were synthesized by replacing the expensive selenourea with elemental selenium powder as an improved selenium precursor. Through ultraviolet-visible spectroscopy, X-ray powder diffraction, inductively coupled plasma emission spectroscopy, elemental analysis, infrared spectroscopy, solid-state nuclear magnetic resonance spectroscopy, DFT theoretical calculations, etc., it was confirmed that they were also (CdSe) 13 MSCs. Reaction stability and increased crystallinity. Afterwards, divalent manganese ions with unpaired electrons were introduced to provide comparison. Through X-ray powder diffraction, ultraviolet-visible light spectroscopy, fluorescence spectroscopy, inductively coupled plasma emission spectroscopy, and X-ray absorption spectroscopy to extend the fine structure, it is known that the synthesis of selenium powder has higher manganese effective doping and emission intensity.The second part extends the optical properties of manganese-doped (CdSe)13 MSCs, and then measures the reflective photoluminescence spectrum and the difference in light emission properties under repeated filling/blocking atmospheres, revealing that oxygen temporarily interferes with manganese light emission and then decreases, and then rises after removing oxygen, forming a reversible fluorescence quenching trend, in order to explore the possible application of phosphorescent semiconductors to gas sensing.The third part uses graphene oxide as a growth template to limit the uniform growth of (CdSe)13 MSC, and to enable effective dispersion of manganese ions. X-ray powder diffraction and ultraviolet-visible light spectroscopy are used to identify through fluorescence spectroscopy, phosphorescence half-lifetime spectroscopy, electron paramagnetic resonance spectroscopy, and electrochemical instrument identification. It is known that the photogenerated carriers of manganese ions are transferred to GO to inhibit electron-hole recombination, resulting in fluorescence quenching and possible photoresponse. It is expected to find the application possibility of semiconductor composite materials.
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硒化鎘, 奈米團簇物, 稀磁性半導體, 氧響應, 氧化石墨烯, 複合材料, cadmium selenide, magic-size clusters, diluted magnetic semiconductors, oxygen sensing, graphene oxide, heterostructure