Journal: Nature Communications

Article Title: Observing growth and interfacial dynamics of nanocrystalline ice in thin amorphous ice films

doi: 10.1038/s41467-024-45234-x

Figure Lengend Snippet: a A schematic of the method for producing amorphous ice films, in which a nanoscale aqueous ice film is plunge-frozen, transferred to a cryo-transfer holder held at 93 K, and placed in a TEM where the temperature was ramped to 143 K. b A schematic for characterizing the growth and interfacial structures of nanocrystalline ice from amorphous ice films with low electron dose. During annealing of the ice film at 143 K, each hole is imaged once before the beam is moved on to the next hole. The experiment allowed the characterization of phases of ice and the associated growth properties. c Representative images of amorphous ice at 93 K, and ice undergoing crystallization at 143 K with increasing annealing time. d Number of ice particles formed from a total of 26 images, with each data point obtained from each image. e Crystallized fraction over time, obtained from a total of 22 images. The Avrami equation is fitted with \documentclass[12pt]{minimal} \usepackage{amsmath} \usepackage{wasysym} \usepackage{amsfonts} \usepackage{amssymb} \usepackage{amsbsy} \usepackage{mathrsfs} \usepackage{upgreek} \setlength{\oddsidemargin}{-69pt} \begin{document}$$\tau=$$\end{document} τ = 354.6 s and \documentclass[12pt]{minimal} \usepackage{amsmath} \usepackage{wasysym} \usepackage{amsfonts} \usepackage{amssymb} \usepackage{amsbsy} \usepackage{mathrsfs} \usepackage{upgreek} \setlength{\oddsidemargin}{-69pt} \begin{document}$$n=$$\end{document} n = 2.88. The shading indicates the stages of crystallization including nucleation (light green), growth (moderate green), and the plateau phase (dark green). f Histogram of ice particle sizes over different time frames, with each histogram corresponding to regions indicated by different color shades in e . The dotted lines represent Gaussian fits, with the orange lines centered at 3500 and the light blue lines centered at 9000 and 9500 for the middle and bottom histograms, respectively. The solid black line represents the sum of the two Gaussian fits. g SAED pattern of amorphous ice at 93 K and h SAED pattern of ice annealed at 143 K, from the same sample but different region as in g . i TEM image (left) and SAED pattern (right) of small, finitely growing ice I c nanocrystals and j TEM image (left) and nanobeam diffraction pattern (right) of a large, continuously growing ice I c+h nanocrystal exhibiting hetero-crystallinity and planar defects, shown by the presence of I h features and streaks in the diffraction pattern. The dotted line in the TEM image delineates an ice nanocrystal domain of interest. k Radially averaged SAED patterns for amorphous ice at 93 K in g (red), ice I c in i (orange), and ice after annealing at 143 K in h (blue). The asterisks mark the unique peaks of ice I h . Simulated XRD data for ice I c (gray) and I h (black) are plotted with 2 θ , which were calibrated from the momentum transfer values. Scale bars for TEM images = 100 nm. Scale bars for diffraction patterns = 2 nm −1 .

Article Snippet: Noise in image is filtered out using a Gaussian filter and feature points were extracted using MATLAB’s built-in detectSURFeatures function.

Techniques: Crystallization Assay

Journal: Nature Communications

Article Title: Observing growth and interfacial dynamics of nanocrystalline ice in thin amorphous ice films

doi: 10.1038/s41467-024-45234-x

Figure Lengend Snippet: a False color time-resolved in-situ TEM images of the first four frames of the growths of P1 and P2, which correspond to ice I c and ice I c+h nanocrystals, respectively. Scale bar = 50 nm. b Intensity profiles of P1 and P2 in sequential frames of the TEM images. P2 shows the presence of a bright-contrast region indicative of low mass-thickness contrast. c Contours of P1 and P2 and d changes in their area over time. Scale bar = 50 nm. e HRTEM image of a heterocrystalline ice domain that includes the surroundings of the domain. Stacking sequences are labeled. f False-colored inverse FFT image, which shows areas that are high in crystallinity as yellow, and areas that are low in crystallinity in purple. Scale bars = 2 nm. g TEM image of a representative continuously-growing ice domain with its interfacial region. The white dashed circle represents the area where the aperture was inserted for SAED analysis. Scale bar = 50 nm. h Diffraction patterns obtained at the aperture area and at amorphous ice at 143 K. i Radial average of the amorphous components of the diffraction patterns in h , with the data points (solid dots) fitted with two Gaussian distributions (solid lines). Scale bar for diffraction patterns = 2 nm −1 .

Article Snippet: Noise in image is filtered out using a Gaussian filter and feature points were extracted using MATLAB’s built-in detectSURFeatures function.

Techniques: In Situ, Labeling