Total X‐Ray Scattering and Small‐Angle X‐ray Scattering for Determining the Structures, Sizes, Shapes, and Aggregation Extents of Iron (Hydr)oxide Nanoparticles

Jun, Young‐Shin; Lee, Byeongdu

doi:10.1002/9783527691395.ch16

Cited by 6 publications

(10 citation statements)

References 75 publications

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“…This observation is contrary to our microscale observation showing significant changes in CaP distribution by the cathode application (Figures 1e−g and 2), emphasizing that multiscale analyses are necessary to understand biomineralization of bonelike hierarchical scaffolds 31,42. With the given morphology (from SAXS fitting) and crystalline structure (from WAXD), the volume fractions of newly formed CaP minerals, f V (Figure3c), can be quantified 24,35,43,44. Compared to the values for the control and anode groups, f V increased by about 38% and 57% from pulsed stimulation applied through the cathode, respectively (p < 0.1, Tukey HSD posthoc test to one-way ANOVA).…”

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confidence: 87%

“…With the given morphology (from SAXS fitting) and crystalline structure (from WAXD), the volume fractions of newly formed CaP minerals, f V (Figure c), can be quantified. ,,, Compared to the values for the control and anode groups, f V increased by about 38% and 57% from pulsed stimulation applied through the cathode, respectively ( p < 0.1, Tukey HSD posthoc test to one-way ANOVA). The f V of samples at the anode were reduced (∼14%) from the control group value, but the difference was within the error range.…”

Section: Resultsmentioning

confidence: 99%

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Pulsed Electrical Stimulation Enhances Body Fluid Transport for Collagen Biomineralization

Kim

Lee

Marshall

et al. 2019

ACS Appl. Bio Mater.

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Mechanical loads from physiologic activities such as walking and running generate bioelectricity in bones. By mimicking bioelectricity, external electrical stimulations have also been used therapeutically to stimulate bone-forming cells and, thus, to promote bone regeneration. However, little is known about the physicochemical mechanism(s) by which electrical stimulations drives calcium phosphate mineralization of collagen. Here, we showed that, during in vitro collagen mineralization in the absence of cells, application of pulsed electrical stimulation significantly enhanced the transport of ionic body fluid components through a micrometer-scale channel (∼100–200 μm gap space between the inner surfaces of tube-like collagen scaffolds and a cathode placed inside the collagen scaffolds). The enhanced transport of ionic precursors increased diffusion of the charged precursors from the channel to the inner collagen surface, where bone mineralization was otherwise restricted. The results indicate that pulsed electrical signals can locally accelerate the nucleation of calcium phosphate nanocrystals in or on collagen, allowing us to better control the spatial distribution of the nanocrystals at the microscale. The findings from this study provide insights into the utilization of electrical stimulation for applications such as facilitating bone-fracture healing and designing better bone-specific biomaterials.

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confidence: 87%

Section: Resultsmentioning

confidence: 99%

Pulsed Electrical Stimulation Enhances Body Fluid Transport for Collagen Biomineralization

Kim

Lee

Marshall

et al. 2019

ACS Appl. Bio Mater.

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“…The scattered X-rays were captured on a Pilatus 2M detector, and lateral scattering intensities within the Yoneda wing were averaged for each q value. ,,, Plots of background-subtracted intensity ( I ) versus q were used to analyze horizontal nuclei sizes as well as the numbers of particles formed on quartz. By fitting the scattering intensity according to nanoparticle’s X-ray scattering theory, ,, we were able to obtain the radius of gyration R g . More details about fitting are included in the Supporting Information.…”

Section: Materials and Methodsmentioning

confidence: 99%

“…A detector 2 m away from the sample cell recorded scattering intensities within a q range of 0.005–0.4 Å –1 , where q is the magnitude of the scattering vector, inversely related to the lateral particle radius R . The scattered X-rays were captured on a Pilatus 2M detector, and lateral scattering intensities within the Yoneda wing were averaged for each q value. ,,, Plots of background-subtracted intensity ( I ) versus q were used to analyze horizontal nuclei sizes as well as the numbers of particles formed on quartz. By fitting the scattering intensity according to nanoparticle’s X-ray scattering theory, ,, we were able to obtain the radius of gyration R g .…”

Section: Materials and Methodsmentioning

confidence: 99%

Salinity-Induced Reduction of Interfacial Energies and Kinetic Factors during Calcium Carbonate Nucleation on Quartz

Jun

2019

J. Phys. Chem. C

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Nucleation is a crucial nanoscale process during the formation of new phases. This study employs CaCO 3 nucleation on quartz as an example system and investigates the effects of salinity on thermodynamic and kinetic factors in CaCO 3 nucleation. In situ grazing incidence small-angle X-ray scattering was used to obtain the nucleation rates of CaCO 3 at different supersaturations (IAP/K sp(calcite) = 10 1.40 to 10 2.00 ) and NaCl-adjusted ionic strengths (i.e., salinities). From a salinity value of 0.15 to 0.85 M, the effective interfacial energy (α) dropped from 48 to 35 mJ/m 2 because of the decrease in water− CaCO 3 and CaCO 3 −quartz interfacial energies, and the kinetic factor was reduced by ∼13 times. Further, high salinity triggered faster nucleation, shorter induction time, and smaller nuclei. Our findings provide new insights for predicting and improving such important processes as CO 2 mineralization during geologic carbon sequestration, desalination membranes, nanoparticle synthesis, and contaminated environments.

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“…The samples were loaded on the beamline stage, SAXS images were obtained. The 1D intensities ( I ) averaged from 2D sample scattering data were subtracted from the averaged background intensities, then plotted as a function of the scattering vector, q , and analyzed by MATLAB based software developed at beamline 12 ID-B. − X-ray PDF measurements were conducted with an energy of 58.290 keV (λ = 0.2127 Å). The same samples used in the SAXS measurements were exposed for 5 s, repeated 36 times for each sample.…”

Section: Methodsmentioning

confidence: 99%

Photochemically-Assisted Synthesis of Birnessite Nanosheets and Their Structural Alteration in the Presence of Pyrophosphate

Jung

Chadha

Min

et al. 2017

ACS Sustainable Chem. Eng.

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Recent findings have showed the environmental abundance of soluble Mn(III)-complexes (e.g., Mn-siderophore and Mn(III)-pyrophosphate (Mn(III)-PP)). Specifically, Mn(III)-PP is of emerging interest in understanding Mn redox cycling and phosphorus cycling in catalysis and environmental systems. Curiously, however, further oxidation of Mn(III)-PP and consequent formation of a MnO2 solid phase have not been considered yet. Here, using photochemically-assisted fast oxidation of Mn2+ (aq) by the reaction with superoxide, generated from nitrate photolysis, we report the role of PP in formation of disordered δ-MnO2 nanosheets and changes in their stacking and structures. With increasing PP concentrations from 0.3 to 2 mM, δ-MnO2 nanosheets showed better stacking (thicker) layers and an alteration from hexagonal to orthogonal structure (more Mn(III) in layers). We found that the amount of Mn(III)-PP complex and the formation rate of δ-MnO2 nanosheets under the different PP concentrations affected both their layer structures and stacking behaviors. These findings open a new possibility of using photochemically-assisted green chemistry to control the properties of disordered δ-MnO2 birnessite nanosheets for use in more effective catalytic reactions, such as water oxidation, and suggest the importance of Mn(III)-PP complexes for the formation of δ-MnO2 nanosheets in nature.

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Total X‐Ray Scattering and Small‐Angle X‐ray Scattering for Determining the Structures, Sizes, Shapes, and Aggregation Extents of Iron (Hydr)oxide Nanoparticles

Cited by 6 publications

References 75 publications

Pulsed Electrical Stimulation Enhances Body Fluid Transport for Collagen Biomineralization

Pulsed Electrical Stimulation Enhances Body Fluid Transport for Collagen Biomineralization

Salinity-Induced Reduction of Interfacial Energies and Kinetic Factors during Calcium Carbonate Nucleation on Quartz

Photochemically-Assisted Synthesis of Birnessite Nanosheets and Their Structural Alteration in the Presence of Pyrophosphate

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