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研究生： 賴洛妘
Lai, Lou-Yun
論文名稱： 以一鍋合成法合成高穩定性之CsPbBr3@孔洞氧化矽螢光材料
One-pot synthesis of highly stable perovskite CsPbBr3 nanoparticle@SiO2 as high-performance phosphor
指導教授： 林弘萍
Ling, Hong-Ping
學位類別： 碩士
Master
系所名稱： 理學院 - 化學系
Department of Chemistry
論文出版年： 2023
畢業學年度： 111
語文別： 中文
論文頁數： 121
中文關鍵詞： 微孔-中孔洞氧化矽 、氧化矽凝膠體 、鈣鈦礦奈米晶體 、螢光材料 、水相一鍋合成法
外文關鍵詞： micro-mesoporous silica, silica gel, perovskite nanocrystals, fluorescent materials
相關次數： 點閱：176  下載：0 
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    • CsPbBr3 全無機型鈣鈦礦作為新世代的發光材料顯示出巨大的潛力，其高光轉換效率、可調發射波長、高色純度和高缺陷容忍度等優異的光學特性，被認為是螢光粉轉換發光二極管中極具前途的替代材料；孔洞氧化矽材料作為載體具有活性位點多、孔洞可調性高、熱穩定性高等優點，因此本研究以此為發想，提出簡易的方法製備高比表面積的孔洞氧化矽載體，應用於 CsPbBr3 複合螢光材料；首先使用有機軟模板輔助氧化矽的縮合聚合反應，藉此控制材料構型，並透過改變溶膠-凝膠反應 pH 值及調整水熱處理時間，合成出不同比表面積和孔徑分布的孔洞氧化矽材料；另以無模板法製備無孔隙的緻密氧化矽凝膠體，透過此簡易環保的方法製備之孔洞氧化矽，可作為高熱穩定性載體應用於各式材料中。
    本研究使用水相一鍋合成法製備 CsPbBr3複合螢光材料，透過此環保的長晶製程在孔洞氧化矽中擔載 CsPbBr3 奈米晶體，使晶粒均勻分散在孔洞中，並以高度交聯的氧化矽凝膠體包覆在外形成保護層，此複合螢光材料具有良好的光致發光效能，以及對水、空氣的穩定性高，材料經過水洗烘乾去除雜質後，即可得到高效能的 CsPbBr3@孔洞氧化矽複合螢光材料，成品也能夠直接以固體粉末的形式做後續應用。此複合螢光材料之光吸收效能良好，能夠在可見光波段 (500 nm 前) 被激發，並於520 nm 處生成一高強度綠色螢光，其螢光放射半高寬最低可達 24.5 nm，螢光量子產率最高達 96 %，螢光放射壽命長達 40.8 ns，並能夠在水中及大氣中長期穩定，未來作為顯示器及二極發光體中之發光材料有極大的潛力。

    CsPbBr3, an all-inorganic perovskite, has demonstrated significant potential as a next-generation luminescent material. Due to its outstanding optical properties, including high light conversion efficiency, tunable wavelength, high color purity, and strong tolerance to defects, it emerges as a promising alternative material for phosphor-converted light-emitting diodes. In this study, we propose a simple method for preparing high surface area micro-mesoporous silica carriers for CsPbBr3 composite fluorescent materials. Organic soft templates are utilized to facilitate the condensation and polymerization of silica, thereby controlling the material structure. By adjusting the pH value of the sol-gel reaction and varying the hydrothermal treatment time, porous silica with different specific surface areas and pore size distributions are synthesized. Additionally, a dense silica gel without pores is prepared using a template-free method. This straightforward and eco-friendly approach to producing micro-mesoporous silica can serve as a highly thermally stable carrier for various materials. For the preparation of CsPbBr3 composite fluorescent materials in this study, an aqueous one-pot synthesis method was employed. CsPbBr3 nanocrystals were encapsulated within the porous silica via an environmentally friendly crystal-growth process. This ensured uniform dispersion of the crystals within the pores, which were subsequently coated with a highly cross-linked silica gel to form a protective layer that exhibits excellent stability against water and air. After thorough washing and drying to remove impurities, the high-performance CsPbBr3@SiO2 composite fluorescent material was obtained. The resulting product can also be directly applied as a solid powder. The composite fluorescent material exhibits high light absorption and can be excited within the visible wavelength range (below 500 nm) to generate intense green fluorescence at 520 nm. It possesses a narrow minimum fluorescence emission line width of 24.5 nm, a maximum fluorescence quantum yield of 96%, and a lifetime of 40.8 ns.

    摘要 I SUMMARY II 致謝 VII 目錄 VIII 表目錄 XII 圖目錄 XIV 第一章 緒論 1 1.1 前言 1 1.1.1 研究動機 2 1.1.2 研究方法 3 1.2 孔洞材料簡介 4 1.3 螢光材料簡介 4 1.3.1 光致發光原理 4 1.3.2 斯托克斯位移與重吸收現象 6 1.3.3 發光量子產率 7 1.3.4 發光衰減壽命 9 第二章 文獻回顧 10 2.1 鈣鈦礦簡介 10 2.1.1 晶相與結構組成 10 2.1.2 能階與光學特性表徵 11 2.2 鈣鈦礦應用 13 2.2.1 電子-電洞分離 13 2.2.2 電子-電洞複合之長壽命發光 15 2.2.3 電子-電洞複合之短壽命發光 18 2.3 純 CsPbBr3 量子點合成 20 2.3.1 熱注射法 20 2.3.2 過飽和再結晶法 21 2.3.3 微波加熱法 22 2.4 保護機制與載體選擇 23 2.4.1 封端配體鈍化 23 2.4.2 無機載體擔載 24 2.4.3 無機模板封裝 25 第三章 實驗方法、儀器及藥品 27 3.1 實驗藥品 27 3.2 實驗儀器 28 3.2.1 掃描式電子顯微鏡 (Scanning Electron Microscopy, SEM) 28 3.2.2 穿透式電子顯微鏡 (Transmission Electron Microscope, TEM) 29 3.2.3 熱重分析儀 (Thermal Gravimetric Analysis, TGA) 30 3.2.4 X-射線繞射儀 (X-Ray Diffractometer, XRD) 31 3.2.5 氮氣等溫吸附-脫附儀 (Nitrogen Adsorption-Desorption Isotherm) 32 3.2.6 螢光光譜儀 (Fluorescence Spectrometer) 36 3.3 實驗方法 38 3.3.1 以軟模板法合成無特定構型之二氧化矽孔洞材料 38 3.3.2 以軟模板法合成囊泡狀之氧化矽孔洞材料 39 3.3.3 以無模板法合成二氧化矽凝膠體 40 3.3.4 製備CsPbBr3@孔洞氧化矽複合螢光材料 41 第四章 製備孔洞氧化矽載體及氧化矽凝膠體材料 42 4.1 微孔-中孔洞氧化矽材料之合成 42 4.1.1 以軟模板法合成之概要 42 4.1.2 反應 pH 值對無特定構型氧化矽材料孔徑分布之影響 45 4.1.3 以不同水熱處理時間調控無特定構型氧化矽材料之孔徑分布 50 4.1.4 軟模板之選擇對合成孔洞氧化矽材料構型之影響 54 4.1.5 在不同溫度下合成囊泡狀孔洞氧化矽對其空腔之影響 56 4.2 以無模板法合成高度交聯之氧化矽凝膠體 59 4.2.1 反應 pH 值對氧化矽凝膠體孔徑分布之影響 60 4.2.2 酸源的挑選對氧化矽凝膠體的影響 61 4.2.3 以不同氧化矽源作為前驅物合成之探討 62 第五章 孔洞氧化矽載體應用於合成 CsPbBr3 複合螢光材料 64 5.1 以一鍋合成法合成 CsPbBr3@孔洞氧化矽複合螢光材料 64 5.1.1 CsPbBr3@孔洞氧化矽複合螢光材料設計與發想 64 5.1.2 CsPbBr3@孔洞氧化矽複合螢光材料之鑑定 66 5.2 探討不同氧化矽凝膠體對螢光材料之包覆效果 69 5.2.1 不同氧化矽前驅物合成之氧化矽凝膠體包覆 69 5.2.2 不同酸源合成之氧化矽凝膠體包覆 72 5.3 水洗複合螢光材料對螢光強度之影響 74 5.4 在不同孔洞氧化矽載體中擔載 CsPbBr3 奈米晶體之探討 80 5.4.1 以矽酸鈉合成之孔洞氧化矽載體 80 5.4.2 以矽酸鋰合成之孔洞氧化矽載體 83 5.4.3 以四乙氧基矽烷合成之孔洞氧化矽載體 85 5.5 CsPbBr3奈米晶體在氧化矽孔洞中生成機制之研究 89 5.5.1 探討氧化矽孔洞對CsPbBr3奈米晶體之錨定作用 91 5.5.2 液相反應 94 5.5.3 固相反應 98 5.6 前驅物添加比例對複合螢光材料之影響 101 5.6.1 孔洞氧化矽載體對氧化矽凝膠體之比例 101 5.6.2 氧化矽總量對 CsBr、PbBr2 之比例 103 5.7 複合螢光材料之光學性質鑑定與穩定性測試 104 5.8 不同鹵素組成對複合螢光材料放光波長之影響 109 第六章 總結論 112 參考文獻 113

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