Analysis of X-ray images and spectra (aXis2000): A toolkit for the analysis of X-ray spectromicroscopy data

Hitchcock, Adam P.

doi:10.1016/j.elspec.2023.147360

Cited by 30 publications

(11 citation statements)

References 37 publications

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“…Five ×5 μm stack images were taken across the carbon K-edge (270 to 350 eV) with 20 spatial points and 100 ms dwell time. All STXM stack images and NEXAFS spectra were analyzed using the aXis2000 software, where the transmitted intensity ( I ) was normalized to an I 0 spectrum (determined from a blank membrane) to get an optical density (OD = log( I 0 / I )) spectrum. These spectra were then background subtracted, smoothed, and normalized to the edge-jump taken as the intensity at 300 eV.…”

Section: Methodsmentioning

confidence: 99%

Blade Coating Poly(3-hexylthiophene): The Importance of Molecular Weight on Thin-Film Microstructures

Dickson,

Cranston,

et al. 2023

ACS Appl. Mater. Interfaces

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Poly(3-hexylthiophene) is one of the most prevalent and promising conjugated polymers for use in organic electronics. However, the deposition of this material in thin films is highly dependent on the process, such as blade coating versus spin coating and material properties such as molecular weight. Typically, large polymer dispersity makes it difficult to isolate the effect of molecular weight without considering a distribution. In this study, we characterize oligothiophenes of exactly 8, 11, and 14 repeat units, which were deposited into thin films by varying blade coating conditions and postdeposition annealing. From synchrotron-based grazing incidence wide-angle X-ray scattering (GIWAXS), scanning transmission X-ray microscopy (STXM) and near-edge X-ray absorption fine structure spectroscopy (NEXAFS), Raman microscopy, optical microscopy, and X-ray diffraction (XRD), it was suggested that higher molecular weight polymers exhibit a fast-forming crystalline polymorph (form-1) while low molecular weight polymers exhibit a slow forming polymorph (form-2) with large domain boundaries. As molecular weight is gradually increased, the polymorph formed transitions from form-1 and form-2, where 11 repeat unit oligomers display both polymorphs. We also found that processing conditions can increase the formation of the form-2 polymorph. We also report improved organic thin film transistor (OTFT) performance when form-1 is present. Overall, oligothiophene polymorph formation is highly dependent on the molecular weight and processing conditions, providing critical insight into the importance of polymer weight control in the development of thin-film electronics based on conjugated polymers.

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Section: Methodsmentioning

confidence: 99%

Blade Coating Poly(3-hexylthiophene): The Importance of Molecular Weight on Thin-Film Microstructures

Dickson,

Cranston,

et al. 2023

ACS Appl. Mater. Interfaces

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“…mcmaster.ca/aXis2000.html). [30] Grazing Incidence Wide-Angle X-Ray Scattering (GIWAXS): GIWAXS measurements were performed at the SIRIUS beamline at the SOLEIL Synchrotron in Saint-Aubin, France. [31] The samples were placed in a chamber that was flushed with helium gas to reduce air scattering.…”

Section: Methodsmentioning

confidence: 99%

Poly(2‐vinylpyridine) as an Additive for Enhancing N‐Type Organic Thin‐Film Transistor Stability

Brixi,

Dindault,

King

et al. 2023

Adv Elect Materials

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N‐type organic semiconductors are particularly susceptible to degradation by ambient air. One such solution to this issue is to include additives in the inks these semiconductors would be cast from that would enhance device stability after film deposition. This method would reduce the number of processing steps needed to fabricate devices compared to other stabilization methods, such as encapsulation. In this study, the stabilization of n‐type performance of the semiconductor poly{[N,N′‐bis(2‐octyldodecyl)‐naphthalene‐1,4,5,8‐bis(dicarboximide)‐2,6‐diyl]‐alt‐5,5′‐(2,29‐bisthiophene)} (P(NDI2OD‐T2)) when it is blended with an increasing proportion by weight of poly(2‐vinylpyridine) (P2VP) is reported. The simple synthesis of P2VP also makes it an ideal candidate material for large‐scale applications. Concentrations as low as 0.1% P2VP incorporated into the P(NDI2OD‐T2) blends provided an immediate stabilization effect, and at 10% and 50%, longer‐term stability after one week is observed.

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“…All STXM data were analyzed using aXis2000 software . The images in a stack typically drift by a few hundred nanometers over a 40–80 eV scan range.…”

Section: Methodsmentioning

confidence: 99%

“…All STXM data were analyzed using aXis2000 software. 63 The images in a stack typically drift by a few hundred nanometers over a 40−80 eV scan range. Therefore, the stacks were aligned to ∼2 nm registry using a Fourier cross-correlation method.…”

Section: Electrodeposition Of Cu Catalyst Particlesmentioning

confidence: 99%

“…The result of an SVD fitting is a set of component maps (spatial distributions), one for each component, along with the residual of the fit. 64 For quantitative analysis, the external reference spectra are converted to an absolute intensity scale, optical density per nm (OD1), 36,63,64 by scaling the spectrum such that the intensity in the pre-edge and far-continuum (>30 eV above the edge) match the elemental response for 1 nm thickness of the known composition and density of the reference material. The latter are calculated using parameters from the Centre for X-ray Optics database [https://henke.lbl.gov/optical_constants/].…”

Section: Electrodeposition Of Cu Catalyst Particlesmentioning

confidence: 99%

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In Situ Studies of Copper-Based CO₂ Reduction Electrocatalysts by Scanning Transmission Soft X-ray Microscopy

Zhang,

Eraky,

Tan

et al. 2023

ACS Nano

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A microfluidic-enabled electrochemical device has been developed to investigate electrochemically active nanomaterials under reaction conditions using in situ scanning transmission soft X-ray microscopy (STXM). In situ STXM measurements were conducted on electrodeposited Cu catalysts under electrochemical CO 2 reduction (CO 2 R) conditions. The study provides detailed, quantitative results about the changes in the morphology and chemical structure of the catalytic nanoparticles as a function of applied potentials. The deposited Cu nanoparticles initially contain both Cu(0) and Cu(I). As an increasingly cathodic potential is applied, the Cu(I) species gradually convert to Cu(0) over the potential range of +0.4 to 0 V versus the reversible hydrogen electrode (V RHE ). During this process, Cu(I) particles of various sizes are converted to metallic Cu at different reaction rates and at slightly different potentials, indicating a degree of heterogeneity in the electrochemical response of discrete particles. At CO 2 R relevant potentials, only metallic Cu is observed, and the morphology of the particles is fairly stable within the spatial resolution limits of STXM (∼40 nm). We also report in situ STXM studies of a working electrode with relatively thick Cu-based electrodeposits. The spatially resolved chemical analysis identifies that Cu-oxide species can persist under CO 2 R conditions, but only when the catalytic nanoparticles are electronically isolated from the working electrode and therefore are catalytically irrelevant. In summary, in situ STXM is presented as a technique to gain advanced morphological and spatially resolved chemical structure insights into electrochemically active nanomaterials, which was used to provide improved understanding regarding Cu nanomaterial catalysts under CO 2 reduction conditions.

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Analysis of X-ray images and spectra (aXis2000): A toolkit for the analysis of X-ray spectromicroscopy data

Cited by 30 publications

References 37 publications

Blade Coating Poly(3-hexylthiophene): The Importance of Molecular Weight on Thin-Film Microstructures

Blade Coating Poly(3-hexylthiophene): The Importance of Molecular Weight on Thin-Film Microstructures

Poly(2‐vinylpyridine) as an Additive for Enhancing N‐Type Organic Thin‐Film Transistor Stability

In Situ Studies of Copper-Based CO₂ Reduction Electrocatalysts by Scanning Transmission Soft X-ray Microscopy

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Analysis of X-ray images and spectra (aXis2000): A toolkit for the analysis of X-ray spectromicroscopy data

Cited by 30 publications

References 37 publications

Blade Coating Poly(3-hexylthiophene): The Importance of Molecular Weight on Thin-Film Microstructures

Blade Coating Poly(3-hexylthiophene): The Importance of Molecular Weight on Thin-Film Microstructures

Poly(2‐vinylpyridine) as an Additive for Enhancing N‐Type Organic Thin‐Film Transistor Stability

In Situ Studies of Copper-Based CO2 Reduction Electrocatalysts by Scanning Transmission Soft X-ray Microscopy

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Product

Resources

About

In Situ Studies of Copper-Based CO₂ Reduction Electrocatalysts by Scanning Transmission Soft X-ray Microscopy