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| 研究生： |
Mohan Lal Meena Mohan Lal Meena |
|---|---|
| 論文名稱： |
磷酸鹽基材用於照明和光催化劑應用: 合成和表徵 Phosphate based materials for lighting and photocatalyst applications: synthesis and characterization |
| 指導教授： |
林昇佃
Shawn D. Lin 呂宗昕 Chung-Hsin Lu |
| 口試委員: |
林昇佃
Shawn D. Lin 江志強 Jyh-Chiang Jiang 胡哲嘉 Chechia Hu 呂宗昕 Chung-Hsin Lu 林皓武 Hao-Wu Lin 丘德威 Te-Wei Chiu |
| 學位類別： |
博士 Doctor |
| 系所名稱： |
工程學院 - 化學工程系 Department of Chemical Engineering |
| 論文出版年： | 2023 |
| 畢業學年度： | 111 |
| 語文別： | 英文 |
| 論文頁數： | 190 |
| 外文關鍵詞： | Single host white light, Eu3+ phosphor, Judd-Ofelt theory |
| 相關次數： | 點閱：150 下載：0 |
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磷酸鹽基材料具有低水溶性、高化學穩定性、高熱穩定性、優異的電荷穩定性、易於以稀土及過渡金屬摻雜、和成本效益高等優點，適合做為製造磷光體/光催化材料的主體。磷酸鹽基材料具有四面體 3-D 矩陣的多樣化結構，因而可作為優異的電荷穩定結構，增加其應用的各種可能性。 此外，通過摻入其他離子和提供廣泛的晶體場環境可以微調此材料的物理及化學性質，以開發用於照明和光催化劑應用的新型材料。本論文研究旨在通過摻雜調整磷酸鹽基材料，並將其應用於UV/NUV 激發之發光體，用於照明和光催化劑應用。
為了提升材料於UV/NUV 區域的吸收，本研究合成並分析Na2Ca1-x-yCexMnyP2O7、Na2Ca1-xEuxP2O7和 NaCa1-xEux(PO3)3 磷酸鹽材料。這些材料在UV至可見光區具有明顯的激發帶。通過選擇不同的主體晶體和摻雜離子來調整材料，可以滿足此材料在照明和光催化應用標準。本研究對摻雜濃度、激發機制、能量轉移、濃度猝滅、熱穩定性和主晶格等因素進行完整檢測，以了解合成磷酸鹽材料的發光特性。
在第一部分工作中，以Na2CaP2O7焦磷酸鹽材料摻雜Ce3+和Mn2+離子作為單相白光螢光粉。在 365 nm 紫外光照射下，摻雜Ce3+ 離子之Na2CaP2O7產生典型的藍色發射不對稱帶，波長位於 415 nm 左右，肩峰在 455 nm 左右。為了獲得白光，再以Mn2+離子摻雜Na2CaP2O7磷酸鹽材料。當 Na2CaP2O7 主體中 Mn2+濃度升高時，對應於Mn2+躍遷的 560 nm 峰的發射強度變強，且位於415 nm 的 Ce3+ 發射隨之變弱。隨著Mn2+濃度的增加，Ce3+相關強度的降低和Mn2+相關強度的相應增加，表明從 Ce3+到Mn2+ 離子的有效能量轉移的可能性。因此Ce3+的藍色發射和Mn2+的橙紅色發射混合在一起從單一主體提供白光，同時具有高活化能值和低熱猝滅行為，使磷酸鹽基螢光粉適用於白光LED。
在第二部分工作中，開發紅色發光螢光粉以提高第一部分中Na2CaP2O焦磷酸鹽材料發出的白光的顏色品質。在 NUV 照射下，Na2Ca1-xEuxP2O7 螢光粉產生Eu3+ 離子f-f 躍遷的發射特徵。為確認 Eu3+ 離子的局部對稱特性，使用JO 理論計算光學躍遷參數。為深入探討了熱穩定性，Na2Ca1-xEuxP2O7螢光粉在 423 K 時表現出顯著的熱穩定性 (90.63%)，測得的活化能為0.26 eV。此外，Na2Ca1-xP2O7:xEu3+ 螢光粉可以與商用綠-藍光螢光粉混合並塗在NUV晶片上以製造白光LED。
第三部分工作為提高紅光發射效率，利用成分三元相圖合成具有紅光發射的銪離子摻雜磷酸鹽螢光粉。所製備的磷酸鹽材料在612 nm附近表現出源自Eu3+f-f躍遷的窄紅光發射。比較不同主體材料，以NaCa(PO3)3 主體表現出最高的發射強度。通過改變Eu3+濃度研究濃度猝滅過程，顯示猝滅受偶極-偶極相互作用控制。 熱穩定性 (90.17%) 顯示與結構剛度有關，如同通過鍵長扭曲指數評估的結果，研究並利用 Judd-Ofelt (JO) 理論研究NaCa(PO3)3磷酸鹽材料中銪離子附近的局部周圍環境。
第三部分工作驗證離子摻雜磷酸鹽材料的光催化應用，摻雜RE的Na2Ca1-xEuxP2O7 磷酸鹽材料在紫外到可見光（~300-530nm）範圍內產生吸收，主峰在 394 nm 左右，Na2Ca1-xEuxP2O7在570-700 nm 範圍內觀察到發射峰，這使得所製備的材料成為潛在的光催化劑。將 Eu3+插入主體中會在禁區內產生多個亞穩態，從而導致光刺激過程的增強，結果表明Na2Ca1-xEuxP2O7 基質不僅可以充當可見光吸收中心，還可以通過為電子或空穴產生新的trapping pool，為光生載流子提供足夠的複合時間，從而增加電荷分離，促進光生載流子的複合以及光催化反應。此種可見光驅動的反應，以水作為可持續氫源，將環境污染物尿素作為電洞捕獲劑，Eu3+摻雜的Na2CaP2O7 磷光體作為光催化劑，能選擇性地將芳香族羧酸轉化為醛。本研究通過光催化處理富含尿素的廢水，以太陽能驅動製備高附加價值之化學品，提供一條轉廢為寶的途徑。
Phosphate based materials are regarded as a suitable host for the manufacture of phosphor/photocatalytic materials because they possess advantages such as ease of preparation with incorporation of RE (rare earth) / TM (transition metal) dopants, low solubility in water, high chemical and thermal stabilities, excellent charge stabilization, and cost-effectiveness. The diverse structure of phosphate-based materials, which has the tetrahedral 3-D matrix, acts as an optimal charge stabilization structure can open up various possibilities for different applications. Besides, their physical/chemical properties can be fine-tuned by incorporating foreign ions and providing extensive crystal field environments to develop novel materials for lighting and photocatalyst applications. This dissertation study aims to tune phosphate-based materials by doping and use it as UV/NUV pumped phosphor for lighting and photocatalyst applications.
For attaining phosphates with strong absorption in UV/NUV region, Na2Ca1-x-yCexMnyP2O7, Na2Ca1-xEuxP2O7, and NaCa1-xEux(PO3)3 phosphate materials are synthesized and characterized in this study. These materials exhibit significant excitation bands in the UV to visible region. The materials can be tuned by selecting different host crystals and dopants to fulfill their criteria for lighting and photocatalytic applications. The factors such as doping concentration, excitation mechanism, energy transfer, concentration quenching, thermal stability, and host lattice were all examined to understand the luminous characteristics of the synthesized phosphate materials.
In the first part, Na2CaP2O7 pyrophosphate materials were doped with Ce3+ and Mn2+ ions for single phase white emitting phosphors. Under 365 nm UV light irradiation, the addition of Ce3+ ion in the Na2CaP2O7 host revealed an asymmetric band with the typical blue emission around 415 nm and a shoulder around 455 nm. To obtain white light, the Mn2+ ion was supplementarily substituted to the Na2CaP2O7 phosphate materials. When the Mn2+ concentration was elevated in the Na2CaP2O7 host, the emission intensity of 560 nm peak corresponding to Mn2+ transition enhanced significantly at the cost of Ce3+ emission of 415 nm. The systematic decrease of Ce3+ intensity and the corresponding increase in the Mn2+ intensity with the increase in Mn2+ concentration indicated the possibility of effective energy transfer from Ce3+ to Mn2+ ions. As a result, the blue emission from Ce3+ and the orange red emission of Mn2+ are mixed to provide white light from a single host along with high value of activation energy and low thermal quenching behavior, making phosphate based phosphors to be suitable for wLEDs.
In the second part, red light emitting phosphors are developed to enhance the color quality of the emitted white light from Na2CaP2O7 pyrophosphate materials in the first part. Under NUV irradiation, the Na2Ca1-xEuxP2O7 phosphors generate the characteristic Eu3+ ion emissions associated with the f-f transitions. To confirm the Eu3+ ion's local symmetry characteristics, the optical transition parameters are calculated using the JO theory. Furthermore, the thermal stability is explored in depth and the prepared Na2Ca1-xEuxP2O7 phosphors demonstrate remarkable thermal stability (90.63 %) at 423 K, with a measured activation energy of 0.26 eV. Moreover, the Na2Ca1-xP2O7:xEu3+ phosphors can be mixed with commercial green-blue emitting phosphors and coated over a NUV chip to fabricate wLED.
In the third part, to enhance the efficacy of red-light emission, Europium ion doped phosphate phosphors with acute red-light emission are synthesized using a compositional ternary phase diagram. The prepared phosphate materials demonstrated narrow red light emissions around 612 nm, originated by Eu3+ f-f transitions. Among various host materials, NaCa(PO3)3 host showed the highest intensity. The concentration quenching process was studied by varying the Eu3+ concentration, and the quenching was governed by dipole-dipole interaction. Thermal stability (90.17 %) was shown to be related to structural rigidity as evaluated by the bond length distortion index. In addition, the Judd-Ofelt (JO) theory was used to examine the local surrounding environment near the europium ion in the NaCa(PO3)3 phosphate material.
RE-doped Na2Ca1-xEuxP2O7 phosphate materials resulted in absorbance in UV to visible light (~300- 530 nm) range with a dominant peak at around 394 nm and the emission peaks of Na2Ca1-xEuxP2O7 are observed in 570- 700 nm range. This makes the prepared materials a potential photocatalyst in the final chapter. The insertion of Eu3+ into the present host creates several metastable states inside the forbidden region and thereby led to the enhancement of the photostimulation process. The results reveal that Na2Ca1-xEuxP2O7 matrix not only can act as visible-light absorption centres, but also provide sufficient recombination time of the photo-generated charge carriers by generating new trapping pool for electrons or holes, which increases the charge separation and promotes the photocatalytic reaction. Thus, a visible-light driven one-step protocol to selectively convert aromatic carboxylic acids to aldehydes with water as the sustainable hydrogen source, environmental pollutant urea as a hole scavenger and Eu3+ doped Na2CaP2O7 phosphor as a viable photocatalyst. The present work provides a waste-to-value route for solar energy driven preparation of valuable fine chemicals by simultaneous photocatalytic treatment of urea-rich wastewater.
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