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研究生： Maina Moses Mburu
Maina Moses Mburu
論文名稱： 利用具有或無氫鍵之聚異戊二烯高分子分選及穩定分散單壁奈米碳管暨其在薄膜電晶體和突觸記憶元件中之應用
Single-Walled Carbon Nanotubes Sorting and Stability Enhancement by Polyisoprene with or without H-bonding and Application in Thin-Film Transistors and Synaptic Memory Devices.
指導教授： 邱昱誠
Yu-Cheng Chiu
口試委員: 江偉宏
Wei-Hung Chiang
葉旻鑫
Min-Hsin Yeh
石健忠
Chien-Chung Shih
李文亞
Wen-Ya Lee
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： 2022
畢業學年度： 110
語文別： 英文
論文頁數： 189
外文關鍵詞： polyisoprene, physical interactions,, PFO, block copolymer, Sorting, SWCNTs, conjugated polymer, SWCNTs, photonic,, electric, fully modulated synaptic TFT device, stable SWCNTs sorting, low molecular weight, conjugated polymer, polyisoprene, H-bonding.
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    • 共軛高分子分選得到具有可調窄手性的單壁奈米碳管 （SWCNT）是近年來最佳方法的方法之一。芴基高分子最常被研究作為分選SWCNT的共軛高分子，因為它們具有優異的相互作用、分散和隔離半導體奈米碳管的能力。高分子主鏈和奈米碳管壁之間的 π-π 相互作用對促進分選起著關鍵作用，因此，共軛部分通常設計於分選的嵌段高分子之主鏈，以保持合適的結構取向和相互作用。然而，目前分選大直徑奈米碳管的高分子局限於具有高分子量（> 10000 Da）和10個或更多碳的烷基側鏈之芴高分子。此外，雖然壽命長和品質高對於元件都至關重要，但在許多研究中都忽略了分選 sc-SWCNT 的穩定性。在本研究中，我們展示如何利用凡得瓦力和氫鍵等物理作用力在低分子量和短烷基側鏈聚芴中實現大直徑 sc-SWCNTs 的分選，從而獲得高純度和穩定的sc-SWCNTs 解決方案，應用於薄膜電晶體和突觸記憶元件之製造。在實驗的第一部分，我們利用了天然橡膠聚異戊二烯 (PI) 的物理作用力，通過合理設計二嵌段高分子，使具有1208個異戊二烯單元的PFO可以顯著增強單壁奈米碳管的分選，並在溶液中維持直徑為~0.83-1.1 nm的窄手性單壁奈米碳管超過一年，實現單壁奈米碳管的分選之高度穩定。在本研究的第二部分中，我們利用在分選過程後，聚 (9,9-二辛基芴)-b-聚異戊二烯 (PF-b-PI) 自發包裹在 SWCNT 周圍的優勢，設計了一種 TFT 突觸裝置，該裝置包括單層狀 PF-b-PI 包裹的 SWCNT，同時提供半導體和駐極體層功能，簡化了元件結構和製造步驟。由於 SWCNTs 強大的電荷載流子遷移率，(~ 11.3 cm2 V-1 s-1) 實現了高輸出電流 (10-4-10-3 A)，並且由於 PF 是一種光活性共軛高分子，該元件可以由光子和電信號調製。在研究的第三部分，證明了具有氫鍵的聚異戊二烯（側鏈）在低 Mw 共軛高分子中誘導有效的分選和優異的溶液穩定性。研究利用聚 (9,9-二辛基芴) (vinyl-PFO, Mw 4500) 及其與聚異戊二烯 (PI) 的高分子用於分選大直徑 SWCNT。從結果來看，沒有引入含氫鍵的側鏈時，高分子並沒有分選效果；聚（2[[（丁基氨基）羰基]氧基]丙烯酸乙酯（PBACO）和PI可使大直徑（1.17 nm）的半導體SWCNT被分選，在低溫4 ℃、-20 ℃和-80 ℃的環境中溶液的sc-SWCNTs可保持穩定一年以上。此外，sc-SWCNTs溶液可以被製成具有高遷移率的雙極電晶體：p型為48 cm2 V-1 s-1，n 型為32 cm2 V-1 s-1，穩定性 > 6000 s。PI-PBACO 物理作用力改善了SWCNTs相互作用並抑制了奈米管的再聚集，從而實現了出色的分選和溶液穩定性。

    The use of Conjugated polymer is currently the best method for selectively sorting single‐walled carbon nanotubes (SWCNTs) with tunable narrow chiralities. Among the conjugated polymers, Fluorene-based (co)polymers are mostly investigated due to their superior ability to interact, disperse, and isolate semiconducting nanotubes. The π – π interaction between the polymer backbone and nanotubes walls plays a key role to facilitate sorting and therefore, conjugated moieties usually form the main chain in the block copolymers designed for sorting to maintain suitable structure orientation and interaction. However, selection of large-diameter nanotubes is only limited to the fluorene polymers with high molecular weight (> 10000 Da), and alkyl side chain of 10 or more carbons. Additionally, though critical for long-life and high-quality devices, stability of the sorted sc-SWCNTs is overlooked in many studies. In the present study, we demonstrate how sorting of large diameter sc-SWCNTs can be achieved in low molecular weight and short alkyl side chains polyfluorene by use of physical forces such as van der Waal forces, and hydrogen bonding, resulting into highly pure and stable sc-SWCNTs solution, that applied in fabrication of thin-film transistors and synaptic memory devices. In the first part of the work, the natural rubber polyisoprene (PI) physical forces are utilized. Through the rational design of diblock copolymer, PFO with ~1208 isoprene units could remarkably enhance SWCNTs sorting and selected few chiralities with a diameter of ~ 0.83 – 1.1 nm in a highly stable solution for more than one year. In the second part of this study, we took advantage of spontaneous wrapping of poly(9,9-dioctylfluorene)-b-polyisoprene (PF-b-PI) around the SWCNTs after sorting process to design a TFT-synaptic device comprising single-layered PF-b-PI-wrapped-SWCNTs, that serves both semiconductor and electret layer functions, simplifying device structure and fabrication procedure. Due to the robust charge carrier mobility of the SWCNTs, (~ 11.3 cm2 V-1 s-1) high output current (10-4 – 10-3 A) was achieved, and since PF is a photoactive conjugated polymer, the device could be modulated by the both photonic and electric signals. In the third part of the study, the effectiveness of polyisoprene with hydrogen-bonding, to induce superior sorting and solution stability in a low Mw conjugated polymer, even when used as a side-chain was demonstrated. Vinyl-terminated poly(9,9-dioctylfluorene) (vinyl-PFO, Mw 4500) and its copolymer with polyisoprene (PI) were investigated for sorting large-diameter SWCNT. From the result, they had no sorting effects but on introduction of hydrogen-bond containing pendant; Poly(2[[(Butylamino)carbonyl]oxy]ethyl-acrylate (PBACO) to the PI moiety, semiconducting nanotubes with large-diameter (1.17 nm) were sorted and the sc-SWCNTs in solution remained stable for over a year and at low temperatures; 4 ℃, −20 ℃ and −80 ℃. Additionally, solution could fabricate ambipolar transistors with high averaged charge carrier mobility; 48 cm2 V-1 s-1 for p-type, and 32 cm2 V-1 s-1 for n-type, with retention stability > 6000 s. The PI-PBACO physical forces improve interaction and inhibit nanotube reaggregation, resulting in superior sorting and solution stability.

    Table of Contents Abstract iv Acknowledgement vi Table of Contents vii List of Abbreviations. x Table of Figures xiii List of Tables xxi 1.0 Introduction 1 1.1. Background 1 1.1.1. SWCNTs Synthesis, classification, and Characterization 1 1.2. Literature Review 3 1.2.1. SWCNTs sorting/purification survey 3 1.3. Motivation 36 1.4. Objectives of the study 39 2.0 The Impacts of Polyisoprene Physical Interactions on Sorting of Single-Wall Carbon Nanotubes 41 2.1. Introduction 41 2.2. Experimental Methods 44 2.2.1. Materials / Chemicals 44 2.2.2. Methods 45 2.2.3. Characterization 45 2.3. Result and Discussion 46 2.3.1. Impact of PI on the dispersion of semiconducting-SWCNTs 46 2.3.2. Diblock copolymer interactions with SWCNTs 57 2.3.3. Stability testing on the sorted small and large-diameter sc-SWCNTs 59 2.3.4. SWCNTs – Thin Film Transistor (TFT) Fabrication 62 2.4. Conclusion 65 3.0 Conjugated Polymer-Wrapped Single-Wall Carbon Nanotubes for High-Mobility Photonic/Electrical Fully Modulated Synaptic Transistor 66 3.1. Introduction 66 3.2. Experimental section 69 3.2.1. Materials 69 3.2.2. Preparation of SWCNT/PF-b-PI solution 69 3.2.3. Device fabrication 70 3.2.4. Device characterization 70 3.3. Results and Discussion 70 3.3. Conclusion 95 4.0 Highly Stable Single-walled Carbon Nanotube Sorting by Random Copolymer of a Low Molecular Weight Conjugated Polymer with Hydrogen bond containing Polyisoprene. 97 4.1. Introduction 97 4.2. Experimental Section 100 4.2.1. Materials 100 4.2.2. Sorting Procedure 101 4.2.3. AFM and TEM samples preparation 101 4.2.4. TFT device preparation 102 4.2.5. Characterization 102 4.3. Results and discussion 102 4.3.1. Polymer Structure Design and the Sorting Effects. 102 4.3.3. Purity Assessment and Morphology of the Sorted sc-SWCNTs 108 4.3.4. Thin-Film Transistor Fabrication and Analysis 111 4.3.5. Formation of Hydrogen-Bonded Supramolecular Structure and its Sorting Effect 114 4.3.6. Stability Testing on the Sorted sc-SWCNTs 116 4.4. Conclusion 122 5.0 General Conclusion and Future Work 124 5.1. General Conclusion 124 5.2. Future Outlooks 125 References 128 Appendices 158  

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