<scp>GISAXS</scp>: A versatile tool to assess structure and self‐assembly kinetics in block copolymer thin films

Smilgies, Detlef‐M.

doi:10.1002/pol.20210244

Cited by 10 publications

(11 citation statements)

References 116 publications

(302 reference statements)

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“…The combination of grazing incidence small-angle and wide-angle X-ray scattering (GISAXS and GIWAXS) is particularly powerful since it provides information about the translational and orientational ordering of NCs in the assembly, respectively. For further details on X-ray scattering methods and analysis we refer the interested reader to recent review by Smilgies . Recent advances in electron microscopy detector technology have enabled acquisition of electron diffraction pattern maps which provide rich information into the crystallographic orientation of each NC in the field of view .…”

Section: Methodsmentioning

confidence: 99%

“…For further details on X-ray scattering methods and analysis we refer the interested reader to recent review by Smilgies. 64 Recent advances in electron microscopy detector technology have enabled acquisition of electron diffraction pattern maps which provide rich information into the crystallographic orientation of each NC in the field of view. 52 In the imaging analysis of SL structures, we advise caution and awareness with regards to selectively focusing the imaging on nicely ordered regions.…”

Section: Background and Contextmentioning

confidence: 99%

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Fundamental Processes and Practical Considerations of Lead Chalcogenide Mesocrystals Formed via Self-Assembly and Directed Attachment of Nanocrystals at a Fluid Interface

et al. 2021

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Significant advances in the synthesis and processing of colloidal nanocrystals have given scientists and engineers access to a vast library of building blocks with precisely defined size, shape, and composition. These materials have inspired exciting prospects to enable bottom-up fabrication of programmable materials with properties by design. Successfully assembling and connecting the building blocks into superstructures in which constituent nanocrystals can purposefully interact requires robust understanding of and control over a complex interplay of dynamic physicochemical processes. Fluid interfaces provide an advantageous experimental workbench to both probe and control these processes. Despite the ostensible simplicity of fabricating nanocrystal assemblies at a fluid interface, sensitivity to processing conditions and limited reproducibility have underscored the complexity of this process. In situ studies have provided mechanistic insights into the competing dynamics of key subprocesses including solvent spreading and evaporation, superlattice formation, ligand detachment kinetics, and nanocrystal attachment. Understanding how these subprocesses influence the complex choreography of self-assembly, structure transformation, and oriented attachment processes presents a rich research challenge. In this context, we present a detailed methodology for self-assembly and attachment of lead chalcogenide nanocrystals at a liquid–gas interface as a model system for the fabrication of mono- and multilayer cubic connected superlattices. We discuss key experimental parameters such as the characteristics of the building blocks and processing conditions and detailed steps from colloidal nanocrystal injection to superlattice transfer. We hope that this Methods/Protocols paper will provide guidance for future advances in the exciting path toward bringing the prospect of nanocrystal-based programmable materials to fruition.

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Section: Methodsmentioning

confidence: 99%

Section: Background and Contextmentioning

confidence: 99%

Fundamental Processes and Practical Considerations of Lead Chalcogenide Mesocrystals Formed via Self-Assembly and Directed Attachment of Nanocrystals at a Fluid Interface

et al. 2021

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“…Fundamental studies of solvent/polymer interaction are essential for understanding self-assembly processes. , Experimental connections between the swollen- and dried-film nanostructures are nontrivial because of the difficulty associated with performing in situ measurements on films in a swollen state. However, carefully designed experiments that employ electron microscopy, grazing incidence small-angle X-ray scattering, neutron scattering, spectroscopic ellipsometry, or AFM can probe the swollen films in situ . ,,,− For example, environmentally controlled AFM can be used to examine the in situ swelling of BP thin films. With this method, direct investigation of swelling kinetics at the limit of single-layer polymer films was possible .…”

Section: Studies Of Bp Thin-film Self-assembly Processesmentioning

confidence: 99%

From Lab to Fab: Enabling Enhanced Control of Block Polymer Thin-Film Nanostructures

Gottlieb

Guliyeva

Epps

2021

ACS Appl. Polym. Mater.

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Block polymer (BP) self-assembly is an ideal approach to generate periodic nanostructures for thin-film applications such as nanolithography, ultrahigh-density memory storage, sensors, and membrane filtration. However, numerous commercial uses require well-ordered nanopatterns and/or precisely controlled domain orientations that can be produced quickly and reliably. In this Spotlight on Applications, advances in BP thin-film fabrication are highlighted including fundamental studies of BP microphase separation, methods to anneal with improved ordering kinetics, and techniques for shear-based directed self-assembly (DSA); the studies discussed represent important steps toward effective large-area manufacturing of nanoscale features. First, combinatorial/gradient and in situ investigations of interfacial energetics, solvent interactions, and DSA are presented because of the unique insights they provide with respect to morphology control. Next, methods to manipulate BP thin-film morphologies by annealing or shear-based DSA are discussed, highlighting key aspects for these approaches: speed, adaptability roll-to-roll compatibility, and BP system versatility. Finally, an overview of some of the challenges that limit the wider adoption of BP thin-film technologies, and several opportunities to overcome these hurdles are considered, such as latent alignment and multistep processing.

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“…14 Techniques such as grazing incidence smallangle X-ray scattering (GISAXS) have been proven to be ideal for characterizing the morphology of self-assembled block copolymer thin films. 15,16 This study incorporates 12 candidate materials from our library into top gate top contact OTFTs with a poly{[N,N′bis(2-octyldodecyl)-naphthalene-1,4,5,8-bis(dicarboximide)-2,6-diyl]-alt-5,5′-(2,2′-bithiophene)} (P(NDI2OD-T2)) semiconductor layer and examines the thin-film morphology of these films through GISAXS and atomic force microscopy (AFM) (Figure 1). Through comparison of the mobile anion We define the polymer names as S-b-(VX-r-PY) where X/Y = the target ratio of chloromethylstyrene (CMS) (converted to VBBI + after initial polymerization) versus poly(ethylene glycol) methyl ether methacrylate (PEGMA) used in the synthesis of the prepolymer.…”

Section: ■ Introductionmentioning

confidence: 99%

“…This interface is crucial to operation of the device by enabling accumulation of charge carriers in the semiconductor, therefore it is essential to understand how the thin-film morphology impacts the device performance . Techniques such as grazing incidence small-angle X-ray scattering (GISAXS) have been proven to be ideal for characterizing the morphology of self-assembled block copolymer thin films. , …”

Section: Introductionmentioning

confidence: 99%

Poly(ionic liquid) Gating Materials for High-Performance Organic Thin-Film Transistors: The Role of Block Copolymer Self-Assembly at the Semiconductor Interface

Brixi

Radford

Tousignant

et al. 2022

ACS Appl. Mater. Interfaces

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The widespread realization of wearable electronics requires printable active materials capable of operating at low voltages. Polymerized ionic liquid (PIL) block copolymers exhibit a thickness-independent double-layer capacitance that makes them a promising gating medium for the development of organic thin-film transistors (OTFTs) with low operating voltages and high switching speed. PIL block copolymer structure and self-assembly can influence ion conductivity and the resulting OTFT performance. In an OTFT, self-assembly of the PIL gate on the semiconducting polymer may differ from bulk self-assembly, which would directly influence electrical double-layer formation. To this end, we used poly{[N,N′-bis(2-octyldodecyl)-naphthalene-1,4,5,8-bis(dicarboximide)-2,6-diyl]-alt-5,5′-(2,2′-bithiophene)} (P(NDI2OD-T2)) as a model semiconductor for our OTFTs, on which our PILs exhibited self-assembly. In this study, we explore this critical interface by grazing-incidence small-angle X-ray scattering (GISAXS) and atomic force microscopy (AFM) of P(NDI2OD-T2) and a series of poly(styrene)-b-poly(1-(4-vinylbenzyl)-3-butylimidazolium-random-poly(ethylene glycol) methyl ether methacrylate) (poly(S)-b-poly(VBBI+[X]-r-PEGMA)) block copolymers with varying PEGMA/VBBI+ ratios and three different mobile anions (where X = TFSI–, PF6 –, or BF4 –). We investigate the thin-film self-assembly of block copolymers as a function of device performance. Overall, a mixed orientation at the interface leads to improved device performance, while predominantly hexagonal packing leads to nonfunctional devices, regardless of the anion present. These PIL gated OTFTs were characterized with a threshold voltage below 1 V, making understanding of their structure–property relationships crucial to enabling the further development of high-performance gating materials.

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GISAXS: A versatile tool to assess structure and self‐assembly kinetics in block copolymer thin films

Cited by 10 publications

References 116 publications

Fundamental Processes and Practical Considerations of Lead Chalcogenide Mesocrystals Formed via Self-Assembly and Directed Attachment of Nanocrystals at a Fluid Interface

Fundamental Processes and Practical Considerations of Lead Chalcogenide Mesocrystals Formed via Self-Assembly and Directed Attachment of Nanocrystals at a Fluid Interface

From Lab to Fab: Enabling Enhanced Control of Block Polymer Thin-Film Nanostructures

Poly(ionic liquid) Gating Materials for High-Performance Organic Thin-Film Transistors: The Role of Block Copolymer Self-Assembly at the Semiconductor Interface

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