Angular X-ray Cross-Correlation Analysis (AXCCA): Basic Concepts and Recent Applications to Soft Matter and Nanomaterials

Zaluzhnyy, Ivan A.; Kurta, Ruslan P.; Scheele, Marcus; Schreiber, Frank; Ostrovskiǐ, B. I.; Vartanyants, Ivan A.

doi:10.3390/ma12213464

Cited by 27 publications

(30 citation statements)

References 116 publications

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“…AXCCA was applied and two‐point cross‐correlation functions (CCFs) for all channels were calculated, according to Equation ()

C (q_{SL}, q_{AL}, normalΔ) = {(⟨⟩, \overset{I}{true} (q_{SL}, φ) \overset{I}{true} (q_{AL}, φ + Δ))}_{φ}

where

\tilde{I} (q_{SL}, φ) = I (q_{SL}, φ) - {(⟨⟩, I false(q_{SL}, φ false))}_{φ}

and I ( q SL ,φ) is an intensity value taken at the point ( q SL ,φ) which are polar coordinates in the detector plane. [ 8,20,21 ] ⟨…⟩ φ denotes averaging over all azimuthal φ angles. q SL correspond to SAXS peaks and q AL to WAXS peaks.…”

Section: Methodsmentioning

confidence: 99%

“…Here, we address these questions by a direct correlation of the structural and electronic properties of SLs composed of electronically coupled lead sulfide (PbS) NCs. We perform X‐ray nanodiffraction and apply angular X‐ray cross‐correlation analysis (AXCCA) [ 8,20,21 ] to characterize the structure of the SLs, which are correlated with electric transport measurements of the same microdomains. By that, we reveal anisotropic charge transport in highly ordered monocrystalline hexagonal‐close‐packed (hcp) PbS NC SLs and find strong evidence for the effect of SL crystallinity on charge transport.…”

Section: Figurementioning

confidence: 99%

“…To study the relative orientation of the NCs inside the SL, we applied AXCCA, [ 20 ] which is based on the analysis of the cross‐correlation functions (CCFs), to the measured scattering data (Figures S10–S12, Supporting Information). We evaluated the CCFs for the SL and AL peaks for both rhcp and bcc structures.…”

Section: Figurementioning

confidence: 99%

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Structure–Transport Correlation Reveals Anisotropic Charge Transport in Coupled PbS Nanocrystal Superlattices

et al. 2020

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The assembly of colloidal semiconductive nanocrystals into highly ordered superlattices predicts novel structure‐related properties by design. However, those structure–property relationships, such as charge transport depending on the structure or even directions of the superlattice, have remained unrevealed so far. Here, electric transport measurements and X‐ray nanodiffraction are performed on self‐assembled lead sulfide nanocrystal superlattices to investigate direction‐dependent charge carrier transport in microscopic domains of these materials. By angular X‐ray cross‐correlation analysis, the structure and orientation of individual superlattices is determined, which are directly correlated with the electronic properties of the same microdomains. By that, strong evidence for the effect of superlattice crystallinity on the electric conductivity is found. Further, anisotropic charge transport in highly ordered monocrystalline domains is revealed, which is attributed to the dominant effect of shortest interparticle distance. This implies that transport anisotropy should be a general feature of weakly coupled nanocrystal superlattices.

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“…AXCCA was applied and two‐point cross‐correlation functions (CCFs) for all channels were calculated, according to Equation ()

C (q_{SL}, q_{AL}, normalΔ) = {(⟨⟩, \overset{I}{true} (q_{SL}, φ) \overset{I}{true} (q_{AL}, φ + Δ))}_{φ}

where

\tilde{I} (q_{SL}, φ) = I (q_{SL}, φ) - {(⟨⟩, I false(q_{SL}, φ false))}_{φ}

Section: Methodsmentioning

confidence: 99%

Section: Figurementioning

confidence: 99%

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Structure–Transport Correlation Reveals Anisotropic Charge Transport in Coupled PbS Nanocrystal Superlattices

et al. 2020

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“…In the case of plasmonic nanoparticles (e.g., Ag, Au) (XCCA). [8][9][10][11][12] Recently, the use of XCCA in structural studies of self-assembled nanoparticles has increased, [8,[13][14][15] including insitu experiments of phase transitions. [16] Form factor measurements in solution provide statistically robust data for particle diameter, shape and dispersity.…”

Section: Introductionmentioning

confidence: 99%

Plasmonic Supercrystals with a Layered Structure Studied by a Combined TEM‐SAXS‐XCCA Approach

Schulz

Westermeier

Dallari

et al. 2020

Adv Materials Inter

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Supercrystals composed of plasmonic nanoparticles constitute a promising material platform for tailored light‐matter interactions. The optimization of their optical properties requires precise syntheses and a detailed structural characterization that addresses not only the basic geometrical parameters but also the degree of order. Herein, plasmonic supercrystals with a well‐defined layered structure are studied by a combined transmission electron microscopy, small‐angle X‐ray scattering and X‐ray cross‐correlation analysis (TEM‐SAXS‐XCCA) approach. It is demonstrated that scanning small‐angle x‐ray scattering (SAXS) data can unambiguously be assigned to the number of crystalline layers by comparison with complementary transmission electron microscopy (TEM) experiments on the same regions of interest. A small but significant increase of the lattice constant with increasing number of layers and a high degree of orientational order irrespective of the number of layers is found. This points to specifics of the supercrystal formation mechanism that could be utilized to improve the control of self‐assembly for supercrystal geometries with subnanometer precision.

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“…An alternative approach to overcome the random particle orientations is a method called correlated X-ray scattering (CXS) (Kam, 1977(Kam, , 1980 [also referred to as fluctuation X-ray scattering (Kam et al, 1981) or angular X-ray cross-correlation analysis (Kurta et al, 2017;Zaluzhnyy et al, 2019)]. CXS is an emerging method employed to recover the structure of an object from X-ray diffraction patterns of a random ensemble of identical objects.…”

Section: Introductionmentioning

confidence: 99%

Characterizing crystalline defects in single nanoparticles from angular correlations of single-shot diffracted X-rays

Niozu

Kumagai

Nishiyama

et al. 2020

Int Union Crystallogr J

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Characterizing and controlling the uniformity of nanoparticles is crucial for their application in science and technology because crystalline defects in the nanoparticles strongly affect their unique properties. Recently, ultra-short and ultra-bright X-ray pulses provided by X-ray free-electron lasers (XFELs) opened up the possibility of structure determination of nanometre-scale matter with Å spatial resolution. However, it is often difficult to reconstruct the 3D structural information from single-shot X-ray diffraction patterns owing to the random orientation of the particles. This report proposes an analysis approach for characterizing defects in nanoparticles using wide-angle X-ray scattering (WAXS) data from free-flying single nanoparticles. The analysis method is based on the concept of correlated X-ray scattering, in which correlations of scattered X-ray are used to recover detailed structural information. WAXS experiments of xenon nanoparticles, or clusters, were conducted at an XFEL facility in Japan by using the SPring-8 Å ngstrom compact free-electron laser (SACLA). Bragg spots in the recorded single-shot X-ray diffraction patterns showed clear angular correlations, which offered significant structural information on the nanoparticles. The experimental angular correlations were reproduced by numerical simulation in which kinematical theory of diffraction was combined with geometric calculations. We also explain the diffuse scattering intensity as being due to the stacking faults in the xenon clusters.

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Angular X-ray Cross-Correlation Analysis (AXCCA): Basic Concepts and Recent Applications to Soft Matter and Nanomaterials

Cited by 27 publications

References 116 publications

Structure–Transport Correlation Reveals Anisotropic Charge Transport in Coupled PbS Nanocrystal Superlattices

Structure–Transport Correlation Reveals Anisotropic Charge Transport in Coupled PbS Nanocrystal Superlattices

Plasmonic Supercrystals with a Layered Structure Studied by a Combined TEM‐SAXS‐XCCA Approach

Characterizing crystalline defects in single nanoparticles from angular correlations of single-shot diffracted X-rays

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