減少新興污染物尤其是水中抗生素污染的負面影響是 21 世紀的主要挑戰之一，光催化作為一種去除頑固污染物很有前途的技術，吸引了世界各地研究人員的關注，石墨碳氮化物 (g-C3N4, CN) 被稱為光催化劑材料，它具有獨特的性能並且能夠在可見光下應用，然而，由於電荷載流子的快速復合，塊狀 CN 的光催化性能很差，因此，本論文的目的是開發剝離 CN 的光催化劑，用於增強可見光驅動和增加多種抗生素的降解。為了實現這一目標，本文採用了兩種策略，首先，採用形態工程來製備高表面積的剝離 CN，然後選擇另一種具有適當能隙位置的半導體材料，使用不同的合成方法成功製備了以鐵酸鋅 (ZnFe2O4, ZFO) 修飾於剝離CN表面之異質結構 (ZFO@CN)，第一種是熱煅燒輔助 (c-ZFO@CN)，另一種是水熱輔助 (h-ZFO@CN)，接著以h-ZFO@CN 奈米複合材在過氧單硫酸鹽 (PMS) 的存在下輔助光催化降解作為模型污染物的環丙沙星 (CIP)。
在這項研究中，使用了兩種不同的前驅物分別是尿素和雙氰胺，通過簡單的煅燒方法合成了剝離 CN，分析其微觀結構、形態、表面積、原子結合、光學和熱學性質， 此外，在 465 nm 可見光照射下，使用 CIP 作為目標抗生素污染物，對 ZFO@CN 奈米複合材的光催化性能進行了評估。結果表明，與原始剝離的 CN 相比，c-ZFO@CN 奈米複合材在CIP的降解中增強了可見光響應和光催化效率，c-ZFO@CN 奈米複合材的光催化性能是原始剝離 CN 的 5 倍。為了解 c-ZFO@CN 奈米複合材的光降解機制，我們進行了 CIP 光催化降解過程中自由基物種的捕獲實驗測試，結果表明c-ZFO@CN 的主要活性物質是 ●O2− 和 h+，為Z 型 c-ZFO@CN 異質結構增強CIP光降解的主要自由基。另一方面，h-ZFO@CN表現出不同的光催化性能。 雖然c-ZFO@CN-2和h-ZFO@CN-2之間的Eg幾乎相似，但是CIP 光降解中c-ZFO@CN-2的光催化性能在30分鐘內是h-ZFO@CN-2的3.4倍，具體來說，c-ZFO@CN-2 的 kobs 高達 0.043 min-1，而 h-ZFO@CN-2 只有0.013 min-1，由於 c-ZFO@CN-2 的 SBET 比 h-ZFO@CN-2 高 1.7 倍，因此 SBET 對於 CIP 去除起著重要作用，為了增強 h-ZFO@CN-2 的光催化活性，使用 PMS 作為氧化劑。
h-ZFO@CN-2/PMS 系統在 30 分鐘內成功展現了 CIP 的高光降解效率（>99%），kobs 為 0.156 min-1，結果表明h-ZFO@CN-2/PMS 系統分別比沒有 PMS 的 h-ZFO@CN-2 和 c-ZFO@CN-2 系統高了 12 倍和 4 倍，h-ZFO@CN-2/PMS系統中CIP光降解的主要ROS為h+、SO4●−和●OH，而 ●O2− 和 1O2 為次要 ROS。 h-ZFO@CN-2/PMS系統在各種環境參數下均具有優異的光降解性能，適用於較寬的pH值範圍。 此外，h-ZFO@CN-2/PMS 系統成功地防止了金屬浸出，從而提供環保的應用。本研究提出了在可見光照射下通過 h-ZFO@CN 的第 II 型異質結構激活 PMS 的新見解， h-ZFO@CN 和 PMS 之間的協同效應在連續 10 個循環後表現出良好的重複使用性和穩定性，對多種新興污染物表現出超過 90% 的光降解能力，同時提出了 CIP 在 h-ZFO@CN-2/PMS 上可能的光降解途徑。
該論文的結果證實了 ZFO@CN 奈米複合材的光催化性能可以通過 ZFO 和剝離CN 之間的異質介面形成，有效地增強可見光驅動的響應和 CIP 的光降解，此外，高效的載流子分離、豐富的活性位點和出色的 PMS 活化可以有效促進抗生素污染物的去除，這些基於 ZFO@CN 的光催化系統可以作為製造金屬氧化物@CN 異質結構的平台，用於水和廢水淨化。

Reducing negative impact of emerging pollutant especially antibiotics pollution in water is one of the biggest challenges in the 21st century. As a promising technology for removal recalcitrant pollutant, photocatalysis has enamoured researcher across the globe. The graphitic carbon nitride (g-C3N4, CN) has known as photocatalyst material which provide unique properties and workable under visible light. However, the photocatalytic performance of bulk CN is dreadful because of rapid charge carrier recombination. Therefore, the aim of this thesis is to develop exfoliated CN based photocatalyst with enhanced visible-light-driven and increased multiple antibiotic products degradation. To achieve this aim, there are two strategies which have been conducted in this thesis. First, the morphological engineering was employed to produce high surface area of exfoliated CN and followed by selecting another semiconductor material with appropriate band gap position. The exfoliated CN-based heterostructures was successfully fabricated with zinc ferrite (ZnFe2O4, ZFO) which decorate on the surface of exfoliated CN (ZFO@CN) using different preparation methods. The first one is thermal calcination-assisted (c-ZFO@CN) and another one is hydrothermal-assisted (h-ZFO@CN). Meanwhile, the h-ZFO@CN nanocomposite was assisted by the presence of peroxymonosulfate (PMS) for photocatalytic degradation of ciprofloxacin (CIP) as model pollutant.
In this study, the exfoliated CN was synthesized by an effortless calcination method using two different precursors namely urea and dicyandiamide. The microstructures, morphologies, surface area, atomic binding, optical and thermal properties were conscientiously characterized. Moreover, the photocatalytic performances were evaluated by using CIP as a targeted antibiotic pollutant over ZFO@CN nanocomposite under 465 nm visible light irradiation. The results showed that the c-ZFO@CN nanocomposite presented enhanced visible light response and photocatalytic efficiency against CIP compared to pristine exfoliated CN. Thereafter, the increasing photocatalytic performance of c-ZFO@CN nanocomposite is 5-fold than pristine exfoliated CN. To understand photodegradation mechanism of c-ZFO@CN nanocomposite, we have conducted trapping experiment and measurement of radical species during photocatalytic degradation of CIP. The result showed that the main active species for c-ZFO@CN are ●O2− and h+ were found to be the primarily responsible radicals for the enhanced photodegradation of CIP over direct Z-scheme c-ZFO@CN heterojunction. On other hand, h-ZFO@CN was exhibited different photocatalytic performance. Although the Eg between c-ZFO@CN-2 and h-ZFO@CN-2 almost similar, however the photocatalytic performance of c-ZFO@CN-2 is 3.4 times higher than h-ZFO@CN-2 within 30 min for CIP photodegradation. Specifically, the kobs of c-ZFO@CN-2 can reach up to 0.043 min-1, while h-ZFO@CN-2 only up to 0.013 min-1. This result reveals that the SBET plays important role for CIP removal due to c-ZFO@CN-2 possess SBET of 1.7-fold higher compared to that of h-ZFO@CN-2. Therefore, to bolster up photocatalytic activity of h-ZFO@CN-2, PMS was employed as oxidizing agent.
The h-ZFO@CN-2/PMS system has successfully exhibited great photodegradation efficiency of CIP (>99%) in 30 min with kobs of 0.156 min-1. This result presents that h-ZFO@CN-2/PMS system is 12 times and 4 times higher than the h-ZFO@CN-2 and c-ZFO@CN-2 system without PMS, respectively. Meanwhile, the main ROS of CIP photodegradation over h-ZFO@CN-2/PMS system were h+, SO4●−, and ●OH. Whereas, ●O2− and 1O2 were the secondary ROS. In addition, the h-ZFO@CN-2/PMS system had excellent photodegradation performance in the various environmental parameters and could apply in wide range of pH. Moreover, the h-ZFO@CN-2/PMS system successfully preserves from metal leaching thus offers environmental-friendly application. This study developed a new insight to activate PMS via type II heterojunction of h-ZFO@CN under visible light irradiation. The synergetic effect between h-ZFO@CN and PMS exhibits great reusability and stability after 10 cycles sequentially as well as more than 90% photodegradation ability for multiple emerging pollutants. The possible photodegradation pathways of CIP over h-ZFO@CN-2/PMS is also proposed.
This thesis result obviously corroborates that the photocatalytic performance of the ZFO@CN nanocomposite can effectively enhance visible-light-driven response and photodegradation of CIP via heterogenous interface formation between ZFO and exfoliated CN. In addition, the efficient charge carrier separation, abundant active site, and exceptional PMS activation could effectively promote removal of antibiotic pollutants. These photocatalytic systems over ZFO@CN can serve as the platform to fabricate metal oxide@CN based heterojunction for water and wastewater purification.

摘要 I
Abstract IV
Acknowledgements VII
Contents IX
List of Figures XII
List of Tables XVIII
Abbreviations, Units, And Symbols XIX
Chapter 1. Introduction 1
1.1. Motivation 1
1.2. Objectives 4
1.3. Thesis outline 5
Chapter 2. Literature Review 6
2.1. The overview of photocatalysis 6
2.1.1. Semiconductor photocatalyst 7
2.1.2. Photocatalyst of CN 12
2.1.3. Synthesis strategies of CN 17
2.1.4. Morphology engineering of CN 20
2.1.5. Application for water purification 22
2.2. Metal Oxide photocatalyst 24
2.2.1. Spinel ferrite photocatalyst 25
2.2.2. Zinc ferrite (ZnFe2O4, ZFO) 28
2.2.3. Synthesis strategies of ZFO 29
2.2.4. Application for water purification 31
2.3. Modification of CN photocatalysts 32
2.3.1. CN-based Heterogeneous photocatalyst 33
2.3.2. Spinel ferrite/CN heterostructures photocatalyst 43
2.3.3. Influence of SR-AOPs in photodegradation reaction 45
2.4. Ciprofloxacin 50
Chapter 3. Methodology 55
3.1. Materials and reagents 55
3.2. Synthesis of bulk CN and exfoliated CN 55
3.3. Synthesis of ZFO 56
3.4. Thermal calcination-assisted synthesis of ZFO@CN nanocomposite (c-ZFO@CN) 56
3.5. Hydrothermal-assisted synthesis of ZFO@CN nanocomposite (h-ZFO@CN) 57
3.6. Characterization 57
3.7. Ciprofloxacin degradation experiments 58
Chapter 4. Results and discussion 60
4.1. Direct Z-scheme c-ZFO@CN nanocomposites heterojunction with enhanced visible-light responsive for ciprofloxacin degradation 60
4.1.1. Characterization of Exfoliated CN 60
4.1.2. Characterization of ZFO 65
4.1.3. Characterization and photocatalytic performance of c-ZFO@CN 67
4.1.3.1. Microstructures of c-ZFO@CN nanocomposites 67
4.1.3.2. Morphology and bandgap of c-ZFO@CN nanocomposites 71
4.1.3.3. Photocatalytic performance of c-ZFO@CN nanocomposite 75
4.1.3.3.1. Effect of initial CIP concentration 78
4.1.3.3.2. Effect of pH 78
4.1.3.3.3. Effect of inorganic anions 79
4.1.3.3.4. Effect of water matrices 81
4.1.3.3.5. Photocatalyst recyclability and stability 82
4.1.3.3.6. Photocatalytic reaction mechanism 85
4.2. Construction of h-ZFO@CN Type-II heterojunction to activate peroxymonosulfate for enhanced multiple antibiotic photodegradation 88
4.2.1. Structural and optical properties 88
4.2.2. Morphology and microstructure of h-ZFO@CN nanocomposite 94
4.2.3. Photodegradation of CIP over h-ZFO@CN/PMS system 98
4.2.3.1. Effect of PMS dosage 102
4.2.3.2. Effect of initial CIP concentrations 102
4.2.3.3. Effect of pH 103
4.2.3.4. Effect of inorganic anions and humic acid 105
4.2.3.5. Real water sample treatment experiment 107
4.2.3.6. Photocatalyst recyclability, stability, and universality 109
4.2.3.7. Possible photocatalytic reaction mechanism 113
4.2.3.8. Identification of the intermediate products 120
Chapter 5. Conclusion and Future perspectives 123
5.1 Conclusion 123
5.2 Future perspectives 125
References 128

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