How to make persistent micelle templates in 24 hours and know it using X-ray scattering

Sarkar, Amrita; Stefik, Morgan

doi:10.1039/c7ta01034f

Cited by 29 publications

(97 citation statements)

References 56 publications

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“…Despite the widespread production and use of nanomaterials, there remains a need for “materials by design” approaches that support predictable and tailored architectures. A challenge with approaches based on equilibration is that all architectural dimensions are subject to the whims of free‐energy minimization, sometimes called “the tyranny of the equilibrium.” Thus equilibrium processing couples changes to the pore size, wall‐thickness, and/or the morphology symmetry …”

Section: Introductionmentioning

confidence: 99%

“…Persistent micelle templates (PMTs) recently emerged as a unique approach to realize isomorphic sample series (constant morphology symmetry) with independent control of each feature size, namely the wall‐thickness and pore size. PMT has advanced to span a wide range of dimensions from mesoporous to macroporous materials . PMT is based on kinetic control where micelle exchange mechanisms are suppressed to preserve a constant micelle diameter (constant template).…”

Section: Introductionmentioning

confidence: 99%

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Full Gamut Wall Tunability from Persistent Micelle Templates via Ex Situ Hydrolysis

Lantz

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Bergh

et al. 2019

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The predictive self‐assembly of tunable nanostructures is of great utility for broad nanomaterial investigations and applications. The use of equilibrium‐based approaches however prevents independent feature size control. Kinetic‐controlled methods such as persistent micelle templates (PMTs) overcome this limitation and maintain constant pore size by imposing a large thermodynamic barrier to chain exchange. Thus, the wall thickness is independently adjusted via addition of material precursors to PMTs. Prior PMT demonstrations added water‐reactive material precursors directly to aqueous micelle solutions. That approach depletes the thermodynamic barrier to chain exchange and thus limits the amount of material added under PMT‐control. Here, an ex situ hydrolysis method is developed for TiO2 that mitigates this depletion of water and nearly decouples materials chemistry from micelle control. This enables the widest reported PMT range (M:T = 1.6–4.0), spanning the gamut from sparse walls to nearly isolated pores with ≈2 Å precision adjustment. This high‐resolution nanomaterial series exhibits monotonic trends where PMT confinement within increasing wall‐thickness leads to larger crystallites and an increasing extent of lithiation, reaching Li0.66TiO2. The increasing extent of lithiation with increasing anatase crystallite dimensions is attributed to the size‐dependent strain mismatch of anatase and bronze polymorph mixtures.

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Full Gamut Wall Tunability from Persistent Micelle Templates via Ex Situ Hydrolysis

Lantz

Clamp

Bergh

et al. 2019

Small

Self Cite

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“…So far, various analytical tools and methods have been facilitated for observing the variations in the structure of materials from molecular scale to micro‐ and macroscales. Precise measurement and in situ observation are beneficial for developing efficient and innovative synthetic routes . A synthetic method of the micelle templating enables one to control porosity and wall thickness of oxides .…”

Section: Introductionmentioning

confidence: 99%

“…A synthetic method of the micelle templating enables one to control porosity and wall thickness of oxides . A small‐angle X‐ray scattering (SAXS) based geometric model is presented to identify the diameter of the micelles as well as wall thickness . The final topography of targeted materials is precisely controlled, including condensation and structural densification.…”

Section: Introductionmentioning

confidence: 99%

“…Precise measurement and in situ observation are beneficial for developinge fficient and innovative synthetic routes. [8][9][10][11][12] As ynthetic method of the micelle templatinge nables one to control porosity and wall thickness of oxides. [8] A small-angle X-ray scattering (SAXS) based geometric model is presented to identify the diameter of the micelles as well as wall thickness.…”

Section: Introductionmentioning

confidence: 99%

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Analytical Understanding of the Materials Design with Well‐Described Shrinkages on Multiscale

Dutta

et al. 2018

Chemistry A European J

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Shrinkages derived from condensation of frameworks are one of the significant steps for fabricating demanded materials having unique morphologies and properties. Enormous efforts have been dedicated to understanding their mechanisms that are quite useful for the materials design. In this context, diversified measuring and observing tools have been facilitated to evaluate structural contractions and corresponding driving forces. All of the investigations are crucial to encourage the utilization of such shrinkages for the precise design of nanomaterials. In this review, we summarize significant works how to analyze shrinkages in multiscale during the synthesis of materials, which will be useful as a follow-up review to our latest contribution. Well-defined porous materials are also selected as a good candidate for understanding well-described shrinkages. This review aims to provide a detailed glimpse of the development of analyses on shrinking behaviors in multiscale for the materials design. Shrinking degree and direction in multiscale, which are driven by condensation of frameworks, are predominant for understanding and/or predicting final nanostructures of materials after shrinkages.

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Nanostructure Dependence of T‐Nb₂O₅ Intercalation Pseudocapacitance Probed Using Tunable Isomorphic Architectures

Bergh

Lokupitiya

Vest

et al. 2020

Adv Funct Materials

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Intercalation pseudocapacitance has emerged as a promising energy storage mechanism that combines the energy density of intercalation materials with the power density of capacitors. Niobium pentoxide was the first material described as exhibiting intercalation pseudocapacitance. The electrochemical kinetics for charging/discharging this material are surface‐limited for a wide range of conditions despite intercalation via diffusion. Investigations of niobium pentoxide nanostructures are diverse and numerous; however, none have yet compared performance while adjusting a single architectural parameter at a time. Such a comparative approach reduces the reliance on models and the associated assumptions when seeking nanostructure–property relationships. Here, a tailored isomorphic series of niobium pentoxide nanostructures with constant pore size and precision tailored wall thickness is examined. The sweep rate at which niobium pentoxide transitions from being surface‐limited to being diffusion‐limited is shown to depend sensitively upon the nanoscale dimensions of the niobium pentoxide architecture. Subsequent experiments probing the independent effects of electrolyte concentration and film thickness unambiguously identify solid‐state lithium diffusion as the dominant diffusion constraint even in samples with just 48.5–67.0 nm thick walls. The resulting architectural dependencies from this type of investigation are critical to enable energy‐dense nanostructures that are tailored to deliver a specific power density.

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How to make persistent micelle templates in 24 hours and know it using X-ray scattering

Abstract: The controlled fabrication of nanoscale materials can enable new behaviors and properties as well as improved performance.

Cited by 29 publications

References 56 publications

Full Gamut Wall Tunability from Persistent Micelle Templates via Ex Situ Hydrolysis

Full Gamut Wall Tunability from Persistent Micelle Templates via Ex Situ Hydrolysis

Analytical Understanding of the Materials Design with Well‐Described Shrinkages on Multiscale

Nanostructure Dependence of T‐Nb₂O₅ Intercalation Pseudocapacitance Probed Using Tunable Isomorphic Architectures

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How to make persistent micelle templates in 24 hours and know it using X-ray scattering

Abstract: The controlled fabrication of nanoscale materials can enable new behaviors and properties as well as improved performance.

Cited by 29 publications

References 56 publications

Full Gamut Wall Tunability from Persistent Micelle Templates via Ex Situ Hydrolysis

Full Gamut Wall Tunability from Persistent Micelle Templates via Ex Situ Hydrolysis

Analytical Understanding of the Materials Design with Well‐Described Shrinkages on Multiscale

Nanostructure Dependence of T‐Nb2O5 Intercalation Pseudocapacitance Probed Using Tunable Isomorphic Architectures

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Nanostructure Dependence of T‐Nb₂O₅ Intercalation Pseudocapacitance Probed Using Tunable Isomorphic Architectures