【摘要】：貴金屬(尤其是Au和Ag)納米材料因其在光學(xué)、電學(xué)、磁學(xué)以及催化等方面表現(xiàn)出的獨特性質(zhì)引起了科學(xué)界廣泛的關(guān)注。尤其在光學(xué)方面,金屬納米顆粒的局域表面等離子體共振(Local surface plasmonic resonance,LSPR)特性已經(jīng)在光學(xué)成像、生物傳感、表面增強光譜等領(lǐng)域被廣泛應(yīng)用。LSPR的關(guān)鍵性能參數(shù)之一是共振吸收峰的位置,它隨金屬納米顆粒的形貌和尺寸而變化。以銀納米顆粒(Ag nanoparticles,Ag NPs)為例,盡管通過已有的實驗方法,人們已經(jīng)獲得了不同形狀和尺寸的Ag NPs,但尚無法精確調(diào)節(jié)它的共振峰位置。針對上述問題,本論文通過改進(jìn)傳統(tǒng)的Ag NPs光化學(xué)合成工藝,建議了一種共振吸收峰精確可調(diào)的Ag NPs合成方案。該方案分兩個步驟:首先用紫外光照射前驅(qū)溶液(以檸檬酸鈉、硝酸銀、光引發(fā)劑I-2959和去離子水按一定比例配制所得),獲得Ag NPs種子溶液;其次再用具有特定波長的LED作為誘導(dǎo)光源,通過光化學(xué)反應(yīng)來制備不同形狀的Ag NPs。我們的創(chuàng)新點是在光化學(xué)反應(yīng)中引入溫控環(huán)節(jié),在特定溫度下,通過控制光照時間來對共振峰的位置精確調(diào)節(jié)。畢業(yè)論文的主要內(nèi)容概括如下:首先,基于傳統(tǒng)光化學(xué)合成工藝,我們獲得了球形、十面體、六邊形、三角形等形狀各異的Ag NPs,并借助透射電子顯微鏡(Transmission Electron Microscope,簡稱TEM)、紫外可見吸收光譜(Ultraviolet-visible spectroscopy,簡稱UV-Vis)等測試手段對合成的Ag NPs的尺度、形貌以及生長機理等進(jìn)行了研究。實驗表明我們獲得的Ag NPs形貌好于文獻(xiàn)報導(dǎo)。其次,以十面體Ag NPs為例,論文實驗驗證了在特定溫度下,通過控制光化學(xué)合成的光照時間,實現(xiàn)Ag NPs共振峰精確可調(diào)的技術(shù)思路。實驗中,我們在不同反應(yīng)溫度(例如30°C、40°C、50°C、60°C和70°C)下合成十面體Ag NPs,發(fā)現(xiàn)在特定的控溫下,合成納米顆粒的共振峰位置λmax隨反應(yīng)時間t增加,線性紅移。因此,能通過控制t來實現(xiàn)λmax的精確調(diào)節(jié)。此外,我們也證實了反應(yīng)溫度的升高,會加快Ag NPs的成核和生長過程,所以較高溫度下生成Ag NPs的速率較快。最后,本論文也采用有限元法,對實驗中出現(xiàn)的共振峰精確可調(diào)現(xiàn)象的物理起源做了數(shù)值模擬分析。結(jié)果證實納米顆粒的粒徑和倒角r等因素造成了前述的共振峰紅移現(xiàn)象。相關(guān)理論工作有助于更好地理解光化學(xué)合成Ag NPs的微觀過程。
[Abstract]:Precious metal (especially Au and Ag) nanomaterials have attracted much attention of the scientific community because of their unique properties in optical, electrical, magnetic and catalytic fields. In particular, in the optical field, the local surface plasmon resonance (Local surface plasmonic resonance,LSPR) characteristics of metal nanoparticles have been applied in optical imaging, biosensors, Surface enhanced spectroscopy is widely used. One of the key parameters of LSPR is the position of resonance absorption peak, which varies with the morphology and size of metal nanoparticles. Taking silver nanoparticles (Ag nanoparticles,Ag NPs) as an example, although different shapes and sizes of Ag NPs, have been obtained through the existing experimental methods, it has not been possible to accurately adjust the position of its resonance peaks. In order to solve the above problems, by improving the traditional photochemical synthesis process of Ag NPs, a precise and adjustable Ag NPs synthesis scheme with resonant absorption peak is proposed in this paper. The scheme is divided into two steps: firstly, Ag NPs seed solution is obtained by ultraviolet irradiation of precursor solution (prepared with sodium citrate, silver nitrate, photoinitiator I, 2959 and deionized water in a certain proportion). Secondly, LED with specific wavelength was used as the induced light source, and Ag NPs. with different shapes was prepared by photochemical reaction. Our innovation is to introduce temperature control into photochemical reaction, and to adjust the position of resonance peak precisely by controlling illumination time at certain temperature. The main contents of the thesis are summarized as follows: firstly, based on the traditional photochemical synthesis process, we obtained spherical, decahedral, hexagonal and triangular Ag NPs, with different shapes and referred to as TEM), by means of transmission electron microscope (Transmission Electron Microscope,). The size, morphology and growth mechanism of the synthesized Ag NPs were studied by UV-vis absorption spectroscopy (Ultraviolet-visible spectroscopy, UV-Vis) and so on. The experimental results show that the morphology of Ag NPs obtained by us is better than that reported in the literature. Secondly, taking decahedron Ag NPs as an example, the technical idea of precisely adjusting the resonance peak of Ag NPs at a specific temperature is verified by controlling the light time of photochemical synthesis. In the experiments, we synthesized decahedral Ag NPs, at different reaction temperatures (for example, 30 擄C, 40 擄C, 50 擄C, 60 擄C and 70 擄C) and found that the position 位 max of the synthesized nanoparticles shifted linearly red with the increase of reaction time t at a specific temperature control. Therefore, the precise adjustment of 位 max can be realized by controlling t. In addition, we also confirmed that the increase of reaction temperature will accelerate the nucleation and growth process of Ag NPs, so the rate of Ag NPs formation is faster at higher temperature. Finally, finite element method (FEM) is used to simulate the physical origin of the exact tunable phenomenon of resonance peaks in the experiment. The results show that the red shift of the resonance peak is caused by the particle size and chamfer r. The related theoretical work is helpful to better understand the microcosmic process of photochemical synthesis of Ag NPs.
【學(xué)位授予單位】：深圳大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2015
【分類號】：TB383.1;O614.122

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