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研究生：	羅之磊 Rosell, Neon Vicente III Bacarro
論文名稱：	二維材料變得容易：關於熔鹽合成硼氮化物和碳氮化物及其廢水處理之應用 2D Materials Made Facile: A Treatise on the Molten Salt Synthesis of Boron and Carbon Nitrides and their Applications for Wastewater Treatment
指導教授：	張高碩 Chang, Kao-Shuo
學位類別：	博士 Doctor
系所名稱：	工學院 - 材料科學及工程學系 Department of Materials Science and Engineering
論文出版年：	2026
畢業學年度：	114
語文別：	英文
論文頁數：	137
中文關鍵詞：	熔鹽合成、六方氮化硼、石墨氮化碳、聚（三嗪酰亞胺）、光催化、超濾
外文關鍵詞：	molten salt synthesis, hBN, gCN, PTI, photocatalysis, ultrafiltration
ORCID：	0000-0002-9176-4932
相關次數：	點閱：9 下載：0
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熔鹽合成法成功製備了結晶碳和氮化硼，二者皆表現出高結晶度和優異的水分散性。我們製備了結晶度極高的結晶聚三嗪酰亞胺（PTI），並首次透過FT-IR光譜的經驗指數證實了這一點。鉀離子在PTI中的插層是該材料研究中的新發現，這可能是其結晶度增強的原因。 PTI奈米片展現出光催化活性，並採用SDS輔助水熱法與P25複合。優化後的PTI-P25複合材料在300 W氙燈照射下能有效降解亞甲基藍（MB）和羅丹明（RhB）染料，在0.8 V飽和甘汞電極（SCE）下實現了0.6%優異的光電轉換效率。
在實驗室規模下簡單的自下而上合成六方氮化硼（hBN）是此材料經驗研究的關鍵進展。值得注意的是，合成的粉末無需額外處理即可表現出親水性。由於其顯著的親水性，hBN被用作超濾膜的主要成分，該超濾膜在過濾過程中能夠攔截99%的羅丹明B（RhB）染料。當hBN與P25混合並經受300 W氙燈照射時，發現其對活性氧敏感，從而形成可重複使用的超濾膜系統。

Molten salt synthesis was successfully used to create crystalline carbon and boron nitrides, both showing high crystallinity and strong water dispersibility. Crystalline poly-(triazine imide) (PTI) with unmatched crystallinity was produced, supported by our first empirically-derived index of FT-IR spectra for the material. Potassium intercalation in PTI, a novel finding for this material, may explain the enhanced crystallinity. PTI nanosheets demonstrated photocatalytic activity and were combined with commercial photocatalytic titanium dioxide (P25) using a sodium dodecyl sulfate (SDS)-assisted hydrothermal method. The optimized PTI-P25 composite effectively degraded methylene blue and Rhodamine B dyes under 300 W Xenon (Xe) lamp exposure and reached a record photo-to-current efficiency of 0.6% at 0.8 volts versus saturated calomel electrode (V SCE).
The facile, bottom-up synthesis of hexagonal boron nitride (hBN) at the laboratory scale represents a key advancement in the empirical research on this material. Remarkably, the as-synthesized powders exhibited hydrophilicity without requiring additional powder treatment. Due to its pronounced water affinity, hBN was employed as a principal component in an ultrafiltration membrane, which demonstrated the capability to reject 99% of rhodamine B dye during filtration. The dye retained on hBN was found to be sensitive to reactive oxygen species when combined with P25 and subjected to 300 W Xe irradiation, resulting in a reusable ultrafiltration membrane system.

摘要 iii
關鍵字: iii
Abstract iv
Keywords: iv
Acknowledgements v
Dedication vii
Table of Contents ix
List of Figures xv
List of Tables xviii
Preface xix
Part I. Introduction and Overview 1
Introduction 3
1	Background and Motivation 3
1.1	Global Water Purification Needs and Technological Challenges 3
1.1.1	Taiwan’s Local Water Needs 4
1.2	Semiconductor Devices for Water Treatment: Photo(electro)catalysis 6
2	Advances in Photocatalytic Materials by CTRL Lab 7
2.1	Combinatorial high-κ Thin-Films Research 7
2.2	Combinatorial Density-Gradient Hydrothermal Research 7
2.3	Heterojunction and Bandgap Engineering 8
2.4	Multifuntional Composites 8
2.5	Relevance 9
3	Technologically Important Elements and the Opportunity for Metal-Free Alternatives 9
3.1	Overview of Key Elemental Abundances in Earth 9
3.2	Recent Advances and Promise of Metal-Free Materials 10
4	Research Accessibility and Impact in the Developing World 11
5	What is ultrafiltration? 11
6	Research Objectives and Scope 12
6.1	Objectives and Scope of the Research 12
6.2	Dissertation Structure 12
6.3	Acknowledgement of prior publication and copyright notice 13
Literature Review 16
1	Poly-Triazine Imide (PTI): The Crystalline Graphitic Carbon Nitride (gCN) 16
1.1	Historical Overview 16
1.2	Structure, Properties, and Known Synthesis Methods 17
1.3	High-Tech Applications 18
1.4	Material Challenges 18
2	Hexagonal Boron Nitride (hBN) 19
2.1	Historical Overview 19
2.2	Structure and Synthesis. 19
2.3	High-Tech Applications 20
2.4	Material Challenges 21
3	Lithium Chloride (LiCl) and Potassium Chloride (KCl): A Deep Eutectic Molten Salt 21
3.1	Key Properties of the LiCl-KCl Binary System 21
3.2	Why Use LiCl-KCl? 21
4	Photocatalysis and Ultrafiltration: Complimentary Technologies for Water Treatment 22
4.1	Ultrafiltration Overview 22
Part II. Experimental 23
Materials and Methods 25
1	Materials and Reagents Used 25
1.1	Working Gases 25
1.2	Solvents used for washing. 25
1.3	Chemicals Used in Experimentation 25
2	List of Fabrication Equipment and Specifications 27
2.1	Tube Furnace and Alumina Boat 27
2.2	Ultracentrifuge 27
2.3	Ultrasonic Bath 28
2.4	Hydrothermal Autoclave and Oven 29
2.5	Spin Coater 29
2.6	Vacuum Filtration System 29
3	Materials Synthesis and Post-Synthesis Protocols 30
3.1	Molten Salt Synthesis of PTI 30
3.2	Molten Salt Synthesis of hBN 31
3.3	Rhodamine B (RhB) Dye Solution Preparation 31
3.4	Composite and Device Fabrication 31
3.4.1	SDS-Assisted Hydrothermal Decoration of P25 Nanoparticles on PTI 31
3.4.2	Fabrication of PTI-P25 Electrochemical Electrodes 32
3.4.3	Fabrication of P25-hBN Ultrafiltration Membranes 32
4	Characterization Methods 33
4.1	Structural (XRD, TEM, SEM, EA) 33
4.1.1	XRD 34
4.1.2	HRTEM 34
4.1.3	SEM 34
4.1.4	Elemental Analysis 34
4.2	Surface Physics and Chemistry 34
4.2.1	XPS 34
4.2.2	BET 35
4.2.3	TEM-EELS 35
4.3	Optical and Electronic 35
4.3.1	UV-Visible Spectroscopy 36
4.3.2	Ultraviolet Photoelectron Spectroscopy (UPS) 37
4.3.3	Fourier-Tranform Infrared Spectroscopy (FT-IR) 37
4.3.4	Raman and Photoluminescence Spectroscopy 38
4.4	Photoelectrochemical Testing of PTI 38
5	Device Setup Performance Testing 38
5.1	Photocatalytic Reactor Setup 38
5.1.1	P25-PTI powders 38
5.1.2	hBN Photocatalytic Membrane Regeneration Tracking 39
6	Computational Techniques Used for Analysis 39
6.1	XRD Analysis 39
6.2	TEM and EELS Analysis 40
6.3	Deconvolution for XPS 40
6.4	Peaks Identification in Raman and Photoluminescence Spectra 40
6.4.1	Raman Peak Indexing and Literature Comparison 40
6.4.2	Approach to Photoluminescence Spectroscopy 41
6.5	Linear Region Determination and Extrapolation for Tauc plots and UPS 41
6.6	Photocatalytic Semiconductor Band Gap Construction 41
6.7	Photocatalytic Degradation Tracking 42
Results and Discussion 44
1	Material and Device Characterizations 44
1.1	Material Properties 44
1.1.1	PTI and (1-x)PTI–xP25 Composites 44
1.1.2	hBN 54
1.2	Device Properties 63
1.2.1	(1-x)PTI–xP25 (x = 23 at.%) 63
1.2.2	hBN-P25/nylon ultrafiltration membrane 65
2	Photocatalytic and Photoelectrochemical Performance of PTI 67
3	Ultrafiltration Membrane Performance of hBN Nanosheets 72
Part III. Conclusions and Future Work 76
Conclusions 78
Future Work 80
1	Immediate Potential Applications 80
1.1	Capture of Rogue Microplastics and Nanomaterials 80
2	Synthesis Equipment Improvements and Scale-up 80
2.1	Switching out the quartz tube 80
2.2	Synthesis Scale-Up 82
References 84
Declaration on the Use of Generative Artificial Intelligence 113
Permitted Institutional Use and Retained Rights 116
                                    

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