溶劑脫層之過渡金屬二硫化物及六方氮化硼應用於製作水處理和氣體分離薄膜

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研究生：	Degu Lere Keshebo Degu Lere Keshebo
論文名稱：	溶劑脫層之過渡金屬二硫化物及六方氮化硼應用於製作水處理和氣體分離薄膜 Solvent based exfoliation of transitional metal dichalcogenides and hexagonal boron nitride for membrane applications: Water treatment and gas separation
指導教授：	胡蒨傑 Chien-Chieh Hu
口試委員:	Juin-Yih Lai Juin-Yih Lai Wei-Song Hung Wei-Song Hung 王志逢 Chih-Feng Wang 蔡協致 Hsieh-Chih Tsai Kueir-Rarn Lee Kueir-Rarn Lee Da Ming Wang Da Ming Wang Ying Ling Liu Ying Ling Liu Chung Tai-shung Chung Tai-shung Chien-Chieh Hu Chien-Chieh Hu
學位類別：	博士 Doctor
系所名稱：	應用科技學院 - 應用科技研究所 Graduate Institute of Applied Science and Technology
論文出版年：	2021
畢業學年度：	109
語文別：	英文
論文頁數：	116
中文關鍵詞：	過渡金屬二硫化物、六方氮化硼、溶劑脫層、二維奈米片、單寧酸、非共價官能化
外文關鍵詞：	Transition metal dichalcogenides, hexagonal boron nitride, solvent exfoliation, 2D nanosheets, tannic acid, noncovalent functionalization
相關次數：	點閱：423 下載：6
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由於工業化和環境汙染，環境永續需要高效能分離薄膜。薄膜在惡劣的環境下操作勢必遭遇薄膜污損、塑化和機械性質不足等急需解決問題。近年來，層狀材料的二維奈米片因其有趣的特性和廣泛的應用潛力而引起了人們的興趣，它們所製作的薄膜在環境方面的應用特別令人著迷。本論文探索經由溶劑脫層法產生二維奈米片和不同方法製作的二維奈米片薄膜的性能。光譜學和顯微技術被用於鑑定脫層的二維奈米片和製備的薄膜。研究的第一部分，溶劑 (NMP) 剝離的 WS2 奈米片被用於提升聚醚碸混合基質超濾薄膜的性能，該薄膜藉由相轉化法製備完成。純水通量、HA 和 BSA 截留率被用於研究嵌入的奈米片對混合基質薄膜的形態和性能的影響。混合奈米片薄膜的水通量從 200 L m-2 h-1bar-1 提高到 360 L m-2 h-1bar-1，溶質截留率分別為 89%提高到 98% (BSA) 和 87% 提高到 98% (HA)。 BSA過濾膜的抗污損分析顯示混合基質膜具有量好的抗污損性能。在研究的第二和第三部分， TA用於對TMDs 和 h-BN 進行簡單、環保的水溶液脫層同時進行非共價鍵官能化改質，TA 不僅是帶負電荷的界面活性劑，由於其雙親特性亦會吸附在分層的 TMD 和 h-BN 的二維納米片上，此特性可有效的使TMD 和 h-BN脫層。在第二部分的研究中，使用正電子湮滅光譜和 XRD分析 WSe2、MoSe2 和 MoS2 層狀薄膜的微觀結構和層間距，探討薄膜的微觀結構與其氣體分離機制的關聯性。研究所製備薄膜的 H2/CO2 分離性能超過了 Robeson upper boubd。比較WSe2 與 MoSe2薄膜的氣體分離效能，用 Mo 代替 W 時薄膜的主要氣體分離機制從分子篩變為 Knudsen 擴散。然而，硫屬元素原子的變化不會影響氣體分離機制。在第三部分研究中，層狀的官能化h-BN 納米片薄膜被用於快速的溶劑傳輸和溶質篩選，所製備的薄膜在水和有機溶劑中極其穩定，並且在溶劑傳輸方面表現出足夠的效率，具有出色的溶質篩選和長期抗污損性能。h-BN 納米片薄膜的溶劑快速傳輸和溶質的充足分離效率可能是由於穩定的奈米片間通道和層狀網絡，這賦予薄膜用於分離和純化發展的有利特性。2D 奈米片改善薄膜性能的原因可能是由於表面積增加、表面特性變化（親水性和表面電荷）、晶格對稱性的變化以及納米片的非共價官能化。因此，溶劑基脫層納米片狀材料製作的薄膜有非常廣闊的應用前景。

Due to current industrialization and environmental constraints, a highly permselective membrane is needed for environmental applications. However, membrane fouling, plasticization, and firmness problems have encountered during operation in harsh working environments. Layered materials in their two dimensional (2D) nanosheets have sparked a lot of interest in recent years due to their intriguing properties and wide variety of potential applications. Their application for membrane to the environmental aspects is fascinating. In this dissertation, solvent based exfoliation of 2D nanosheets and different avenues to synthesis membranes in a facial way applied. The exfoliated nanosheets and prepared membranes were characterized using spectroscopic and microscopic techniques. In the first approach, solvent N-methyl-2-pyrrolidone exfoliated nanosheets of WS2 used to improve performance of polyethersulfone mixed matrix ultrafiltration membrane, which was prepared via in phase inversion method. The effect of the embedded nanosheets on morphology and performance of the fabricated membrane investigated in terms of pure water flux, humic acid (HA) and bovine serum albumin (BSA) rejection. The water flux improved from 200 L m-2 h-1bar-1 to 360 L m-2 h-1bar-1 with the solutes rejection 89 to 98 % (BSA) and 87 to 98 (HA) after blending of nanosheets. Fouling resistance of the membranes for BSA filtration revealed that mixed matrix membrane has the best antifouling property. In the second and third approach, a simple, environmental-friendly aqueous exfoliation and noncovalent functionalization of transition metal dichalcogenides (TMDs) and hexagonal boron nitride (h-BN) were applied using tannic acid (TA) for laminar membranes synthesis. To delaminate bulk TMD and h-BN efficiently, TA is not only serves as a negatively charged surfactant but also adsorbs to the delaminated 2D nanosheets of TMD and h-BN owing to its amphiphilic nature. In the second application, the microstructure and interlayer spacing of WSe2, MoSe2, and MoS2 laminar membranes were explored using positron annihilation spectroscopy and X-ray diffraction to correlate membrane with their gas transport mechanism. The H2/CO2 separation performance of the resultant membranes surpasses the Robeson’s upper bound. On comparison of WSe2 with MoSe2, replacing W with Mo changes the dominative gas transport mechanism of the membrane from molecular sieving to Knudsen diffusion. However, a change in the chalcogen atom do not affect the gas transport mechanism. In third application, the functionalized exfoliated h-BN nanosheets laminar membrane used for ultrafast solvent transport and solutes screening. Fascinatingly, the membrane produced is extremely stable in both water and organic solvents, and it transports solvents with enough efficiency, effective solute screening, and long-term antifouling performance. The robust nanochannel and thin laminar networks of the nanosheets give the membrane with favorable qualities for separation and decontamination processes, which may explain the membrane's rapid transport of solvents and high separation efficiency of solutes. The improved performance of membrane using 2D nanosheets may be due to increased surface area, change surface chemistry (hydrophilicity and surface charge), change in lattice symmetry, and noncovalent functionalization of nanosheets. Herein, membrane applications of solvent-based exfoliated nanosheets of layered materials are promising.

Contents                                               page
Acknowledgements    v
Abstract    vi
Table of Contents    x
List of figures    xiii
List of tables    xviii
List of symbols and abbreviations    xix
Chapter 1  Introduction    1
1 Why membranes and 2D nanosheets?    1
2 Motivation and objectives    4
3 Thesis organization and general relationship among the three subjects.    6
Chapter 2  Literature review    8
1 Preparation and application of membranes    8
2 Properties of 2D layered materials    9
3 Synthesis of 2D layered naonsheets    10
3.1 Bottom-up approach    11
3.2 Top-down approach    12
4 Membrane synthesis from 2D nanosheets    16
5 Membrane application of 2D nanosheets    17
5.1 TMDs and h-BN nanosheets membrane for water treatment and organic solvent filtration.    17
5.2 TMDs nanosheets membrane for gas separation    23
Chapter 3 Solvent-exfoliated 2D WS2 for improved performance of polyethersulfone mixed-matrix ultrafiltration membrane for water treatment    27
1 Introduction    27
2 Experimental Methods    28
2.1 Materials    28
2.2 Sonication-assisted WS2 liquid phase exfoliation    28
2.3 Characterization of exfoliated tungsten disulfide (E-WS2) 2D nanosheets  and    membrane    29
2.4 Preparation of PES/ WS2 2D nanosheets mixed matrix membrane    30
2.5 Evaluation of separation performance    30
2.6 Anti-fouling of mixed matrix and pristine membranes    31
3 Result and discussion    32
3.1 Exfoliation and characterization of WS2 2D nanosheets    32
3.2. Membrane characterisation    34
3.3 Filtration performance of membranes    36
4 Conclusions    45
Chapter 4  Effect of composition of tannic acid assisted aqueous exfoliated 2D naosheets transitional metal dichalcogenides membranes in hydrogen separation mechanism.    46
1 Introduction    46
2 Materials and methods    47
2.1 Materials    47
2.2 Tannic acid assisted aqueous exfoliation of TMDs.    47
2.3 Characterization of 2D nanosheets    49
2.4 Membrane characterization    49
2.5 Interspace analysis of TMDs nanosheets membranes    50
2. 6 Gas permeation measurements    50
3 Result and discussion    52
3.1 Exfoliation and characterization    52
3.2 Membrane preparation    62
3.3 Gas transport results    65
4 Conclusions    72
Chapter 5  Simultaneous exfoliation and functionalization of hexagonal boron nitride in aqueous phase for ultrafast solvent transport of molecular solute screening membrane.    73
1 Introduction    73
2 Experimental section    74
2.1 Materials    74
2.2 Exfoliation of non-covalent functionalized hexagonal boron nitride nanosheets and     membrane preparation.    75
2.3 Characterization of exfoliated nanosheets and membrane    76
2.4 Assessment of separation performance.    76
3 Result and discussion    77
3.1 Exfoliation and nanosheet characterization    77
3.2 Membrane synthesis and characterization.    87
3.4 Membrane stability on different supports.    89
3.5 Solvent permeance and separation performance of f-BNNs membrane.    94
4 Conclusion    100
Chapter 6  General conclusions and future perspective    101
1 General conclusions    101
2 Future perspective    103
References    104
Publications    115


                                

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