嵌段共聚物微胞於類膠體粒子領域之自組裝行為研究

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研究生：	巴克諾理 Nouri, Babak
論文名稱：	嵌段共聚物微胞於類膠體粒子領域之自組裝行為研究 Self-assembly of block copolymer micelles in the fuzzy colloid regime
指導教授：	陳信龍 Chen, Hsin-Lung
口試委員:	蘇安仲 Su, An-Chung 蔣酉旺 Chiang, Yeo-Wan 孫亞賢 Sun, Ya-Sen 朱哲毅 Chu, Che-Yi
學位類別：	博士 Doctor
系所名稱：	工學院 - 化學工程學系 Department of Chemical Engineering
論文出版年：	2022
畢業學年度：	111
語文別：	英文
論文頁數：	137
中文關鍵詞：	嵌段共聚物、微胞、拉維斯C14相、晶格排列、尺寸分散性
外文關鍵詞：	block copolymer, micelle, Laves C14 phase, lattice packing, size polysispersity
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組成高度不對稱的嵌段共聚物可以微相分離成球狀的微胞結構，微胞之間互斥作用力誘導微胞排列形成晶格結構。近年Frank-Kasper (FK) 相以及準晶結構的發現，嵌段共聚物微胞的堆積結構與機制引起了高度關注，FK相含有至少兩種以上配位數的Voronoi cell。因此，嵌段共聚物微胞在無序排列之微胞相過形成FK相的過程中，微胞尺寸應由單一分佈轉變為多重分佈，此程序需由微胞間的分子質量傳遞來達成。
本研究開創了一種「模糊膠體粒子」的觀念來建構嵌段共聚物之FK相，我們在低於P2VP以的玻璃轉化溫度(T¬gcore)的條件下，限制共聚物分子的質量傳遞，透過長時間退火誘導P2VP-b-PDMS由類液態堆積相(LLP)轉化為Laves C14相。我們使用數種熱處理條件來產生不同平均尺寸及尺寸分散性的P2VP-b-PDMS微胞，形成各種LLP結構，我們發現，經過低於Tgcore的長時間退火可以誘導不同的LLP相轉化為體心立方結構(BCC)或C14結構可，即尺寸分布較均一的微胞傾向堆積成由單一種Voronoi cell構成的BCC結構；而尺寸分布較寬廣的微胞則傾向形成由三種Voronoi cell構成的Laves C14相。
我們進一步針對微胞周遭局部環境進行實空間的分析，發現C14相可以容納較廣泛的粒子間距，並具有較不均一的局部環境。尺寸分布較廣的微胞形成C14相可使外圍之PDMS鏈段的熵損耗較為緩和。原則上，適當的微胞尺寸分散性有利於Laves C14相的形成。我們認為，尺寸分餾是LLP相轉化為C14相的關鍵，即為尺寸分布較廣的粒子可以分餾成三種尺寸次分佈，而排列成C14晶格，這些晶格結構的有序-無序轉化溫度(TODT)與LLP的結構息息相關。最後，我們發現P2VP-b-PDMS的相轉化行為有高度的記憶效應，將樣品升溫到無序微胞結構後淬火，可以回復到原始LLP相的特性。而後在模糊膠體粒子區域進行退火後，即可得到原始的有序結構。

Microphase separation between the constituent blocks of block copolymer (bcp) can generate spherical micelles at large compositional asymmetry. The interaction between the micelles, which is usually repulsive in nature, leads to their organization into long-range ordered lattices. The packing problem of bcp micelles has triggered considerable attention recently by the discovery of Frank-Kasper (FK) phase and quasicrystals. FK phase is the tetrahedrally close packed structure constructed by the distorted icosahedra with the coordination number of 12, 14, 15 or 16 in the unit cell, where each FK phase composes of at least two types of these motifs. In principle, the formation of FK phase from the supercooled liquid phase of bcp micelles should involve the mass transport of the constituent molecules to transform the unimodal distribution of micelle size into the multimodal distribution prescribed by the volume asymmetry of the Voronoi cells in the FK phase. Here we present a so-called “fuzzy colloid regime” in which the Laves C14 phase of a pol(2-vinyl pyridine)-block-poly(dimethyl siloxane) (P2VP-b-PDMS) developed from the liquidlike packing phase (LLP) below the glass transition temperature of the micelle core (T¬gcore) formed by P2VP block, where the mass transport mechanism was inaccessible.
Several thermal processing conditions were adopted to produce the P2VP-b-PDMS micelles forming various LLP structures with different average micelle sizes and size dispersity. Prolonged annealing of these LLP phases at T < Tgcore was found to yield body-centered cubic (BCC) or C14 phase depending on the LLP structure. Micelles with narrow size dispersity tended to pack into BCC lattice composed of one type of Voronoi cell, while the broadly distributed micelles were found to pack into Laves C14 phase comprising three types of Voronoi cells. The real-space analysis of the local environments of the particles revealed that C14 phase can accommodate the particles with a broader range of interparticle distance and less uniform local environment, such that the PDMS coronal blocks of the micelles with greater size dispersity suffered a lower degree of packing frustration when they organized into C14 lattice. In principle, polydispersity destabilizes the classical lattice structure; however, a modest degree of polydispersity causes symmetry breaking, leading to the formation of Laves C14 phase.
We propose that a self-sorting process via size fractionation was operative to direct the effective development of C14 phase from the LLP phase with sufficiently large size dispersity. The fractionation took place to yield three fractions of particles from the parent distribution with their relative populations approximately followed the stoichiometry of the particles in the C14 unit cell. Due to the metastable nature of the ordered phases, their order-disorder transition temperatures (TODTs) were found to depend strongly on the structures of the LLP phases from which they developed. Finally, we revealed a strong memory effect underlying the phase transitions. Heating the samples to the DM phase followed by quenching effectively recovered the characteristics of the original LLP phase from which the ordered phase evolved. The subsequent annealing in the fuzzy colloid regime led to the formation of the ordered phase identical to the original one. The present research lands a new paradigm of bcp metallurgy where the micelles can find their optimum ordered packing under a predetermined state of distribution without adjusting their sizes.

Table of content
Abstract...........................................................................................................I
Table of content.............................................................................................III
List of figures..................................................................................................V
List of tables....................................................................................................X
Chapter 1. Introduction ....................................................................................1
1.1 Background of Research ..................................................................................1
1.2. Quasicrystal and FK phases of one-component linear block copolymers......5
1.2.1. Conformational asymmetry effect on the stability of Frank-Kasper
phase .....................................................................................7
1.2.2. Frank-Kasper phase of block copolymer with architectural
asymmetry ...........................................................................13
1.3. Frank- Kasper phase of block copolymer blend systems..............................16
1.3.1. Block copolymer/block copolymer blends forming Frank-Kasper
phase ...................................................................................17
1.3.2. Frank-Kasper phase of block copolymer /homopolymer blends......18
1.4. Self-assembly of colloidal suspension..........................................................22
1.4.1. Nanoparticle interactions .........................................................23
1.4.2. Hard-core van der Waals interaction ..........................................23
1.5. Self-assembly of binary hard particle suspension: effect of polydispersity .31
1.5.1. Size disparity effect of ligand-coated hard particles......................34
1.6. Conclusions and outlook...............................................................................36
1.6. Objectives of research and overview of thesis..............................................38
1.7. References and notes.....................................................................................42
Chapter 2. Emergence of a metastable Laves C14 phase of block copolymer micelle
bearing glassy core .........................................................................................63
2.1. Introduction...................................................................................................63
IV
2.2. Experimental Section....................................................................................66
2.2.1. Sample preparation .................................................................66
2.2.2. Rheological measurement ........................................................67
2.2.3. Synchrotron small angle X-ray scattering (SAXS) measurements...68
2.3. Results and Discussion .................................................................................69
2.3.1. Glass transition temperature and the conformational asymmetry
parameter of the P2VP-b-PDMS..............................................69
2.3.2. Micelle ordering resolved by SAXS...........................................71
2.3.3. Thermodynamic argument of the micelle ordering from the LLP phases
...........................................................................................79
2.3.4. Order-disorder transition of the metastable C14 phase ..................82
2.4. Conclusion ....................................................................................................84
2.5. References and notes.....................................................................................86
Chapter 3 Phase control of colloid-like block copolymer micelles by tuning size
distribution via thermal processing..................................................................95
3.1. Introduction...................................................................................................95
3.2. Results and discussion ..................................................................................99
3.2.1. The LLP phases generated by different thermal processing conditions
and the impact of LLP structure on the micelle ordering behavior in
the fuzzy colloid regime .........................................................99
3.2.2. The local environment and the particle size dispersity of the LLP
phases that favor the formation of Laves phase ........................106
3.2.3. The self-sorting mechanism leading to the development of C14 phase
from the LLP phase .............................................................111
3.2.4 The order-disorder transition of the metastable ordered phases......118
3.3. Conclusions.................................................................................................122
3.4. References and notes...................................................................................125
Chapter 4 Overall Summery and Suggestion for Future Work .........................132
List of Publications.......................................................................................136
                                

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