Elementary steps at the surface of ice crystals visualized by advanced optical microscopy

Sazaki, Gen; Zepeda, Salvador; Nakatsubo, Shunichi; Yokoyama, Etsuro; Furukawa, Yoshinori

doi:10.1073/pnas.1008866107

Cited by 110 publications

(162 citation statements)

References 46 publications

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“…Hence, the β-QLL cannot be a solid phase but is a quasi-liquid phase appearing below 0°C. In the second case, the β-QLL has to be easily deformed by the lateral movement of elementary steps that are only 0.37 nm thick (7). Such an easily deformed phase would be a quasi liquid, rather than a solid, although at present the rigidity of a solid ice film of nanometer thickness is unclear.…”

Section: Resultsmentioning

confidence: 99%

“…We attached a confocal system (FV300; Olympus Corporation) to an inverted optical microscope (IX70; Olympus Corporation), as previously explained (6,7). A superluminescent diode (Amonics Ltd.; model ASLD68-050-B-FA: 680 nm) and a He-Ne laser (Melles Griot 05-LHP-991: 633 nm) were used for LCM-DIM and interferometric observations, respectively.…”

Section: Methodsmentioning

confidence: 99%

“…We and Olympus Engineering Co., Ltd. have developed one such technique-namely, laser confocal microscopy combined with differential interference contrast microscopy (LCM-DIM) (6), which can directly visualize the 0.37-nm-thick elementary steps on ice crystal surfaces with a typical frame rate of 0.1-4 s per frame (7). In this study, we directly visualized surface melting processes on ice crystal surfaces to elucidate the dynamic behavior of QLLs and found that QLLs are made up of two different phases (Fig.…”

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confidence: 99%

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Quasi-liquid layers on ice crystal surfaces are made up of two different phases

Sazaki

Zepeda

Nakatsubo

et al. 2012

Proc. Natl. Acad. Sci. U.S.A.

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109

128

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Ice plays crucially important roles in various phenomena because of its abundance on Earth. However, revealing the dynamic behavior of quasi-liquid layers (QLLs), which governs the surface properties of ice crystals at temperatures near the melting point, remains an experimental challenge. Here we show that two types of QLL phases appear that exhibit different morphologies and dynamics. We directly visualized the two types of QLLs on ice crystal surfaces by advanced optical microscopy, which can visualize the individual 0.37-nm-thick elementary steps on ice crystal surfaces. We found that they had different stabilities and different interactions with ice crystal surfaces. The two immiscible QLL phases appeared heterogeneously, moved around, and coalesced dynamically on ice crystal surfaces. This picture of surface melting is quite different from the conventional picture in which one QLL phase appears uniformly on ice crystal surfaces.in situ observation | laser confocal microscopy | differential interference contrast microscopy

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Section: Resultsmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

mentioning

confidence: 99%

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Quasi-liquid layers on ice crystal surfaces are made up of two different phases

Sazaki

Zepeda

Nakatsubo

et al. 2012

Proc. Natl. Acad. Sci. U.S.A.

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109

128

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“…Additionally, evidence of dissolution of the f010g face in contact with water sample Naica-08 was found at 45°C (during an experimental run of 20 h the opening of an etch pit on the f010g face was observed). Currently we are precisely determining the dissolution temperature interval for gypsum in Naica waters with laser confocal differential interference contrast microscopy (3,22). Although growth of gypsum crystals above 60°C in the Naica caves is very unlikely, normal growth rates were also measured at: 65, 70, 80, and 90°C because additional measurements should allow a better fit of the growth rates in the temperature range of interest (50-60°C, see next section).…”

Section: Geologymentioning

confidence: 99%

Ultraslow growth rates of giant gypsum crystals

Driessche

García-Ruiz

Tsukamoto

et al. 2011

Proc. Natl. Acad. Sci. U.S.A.

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Mineralogical processes taking place close to equilibrium, or with very slow kinetics, are difficult to quantify precisely. The determination of ultraslow dissolution/precipitation rates would reveal characteristic timing associated with these processes that are important at geological scale. We have designed an advanced high-resolution white-beam phase-shift interferometry microscope to measure growth rates of crystals at very low supersaturation values. To test this technique, we have selected the giant gypsum crystals of Naica ore mines in Chihuahua, Mexico, a challenging subject in mineral formation. They are thought to form by a self-feeding mechanism driven by solution-mediated anhydritegypsum phase transition, and therefore they must be the result of an extremely slow crystallization process close to equilibrium. To calculate the formation time of these crystals we have measured the growth rates of the f010g face of gypsum growing from current Naica waters at different temperatures. The slowest measurable growth rate was found at 55°C, 1.4 AE 0.2 × 10 −5 nm∕s, the slowest directly measured normal growth rate for any crystal growth process. At higher temperatures, growth rates increase exponentially because of decreasing gypsum solubility and higher kinetic coefficient. At 50°C neither growth nor dissolution was observed indicating that growth of giant crystals of gypsum occurred at Naica between 58°C (gypsum/anhydrite transition temperature) and the current temperature of Naica waters, confirming formation temperatures determined from fluid inclusion studies. Our results demonstrate the usefulness of applying advanced optical techniques in laboratory experiments to gain a better understanding of crystal growth processes occurring at a geological timescale.phase shifting interferometry | mineral growth D uring the last decade, the field of mineral growth has experienced important advances in analytical instrumentation (1). The development of state-of-the-art methods for nanometric observation, such as high-resolution atomic force microscopy (2), or advanced optical microscopy techniques like laser confocal differential interference contrast microscopy (3) and phase-shift interferometry (4, 5), have allowed the study at nanoscopic levels of the different growth mechanisms exhibited by crystals, emphasizing the direct relation between the morphology and the growth processes taking place on each crystal face. For example, the application of in situ nanoscale observation of calcite crystal growth in the lab have revealed the microscopic causes of the large morphological variety exhibited by natural occurring calcite crystals (6-8). These, and other works (9-11) have demonstrated the power of laboratory crystal growth studies for sharpening the picture of crystallization occurring in nature.Recently, a very striking crystal growth problem in earth sciences has emerged: the existence of giant crystals of gypsum (CaSO 4 :2H 2 O), in particular those found in the range of Naica, Mexico (12, 13). Large gypsum cryst...

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“…Before and after the single-molecule visualization, the surface morphology of a monoclinic HEWL crystal ( Figure 3a) was observed by laser confocal microscopy combined with differential interference contrast microscopy (LCM-DIM), by which at first elementary steps on protein crystal surfaces (several nanometers in height) 14 and later elementary steps on ice crystal surfaces (0.37 nm in height) 15 can be visualized with sufficient contrast. From the in situ observation of elementary steps on a monoclinic HEWL crystal by LCM-DIM, we confirmed that elementary steps were not proceeding or receding, proving that a crystal had been maintained in the equilibrium condition during the single-molecule visualization.…”

Section: Methodsmentioning

confidence: 99%

Attachment and Detachment Processes of Individual Lysozyme Molecules on a Surface of a Monoclinic Lysozyme Crystal Studied by Fluorescent Single-Molecule Visualization

Dai

Zheng

Sazaki

et al. 2014

Crystal Growth & Design

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On a {101̅ } face of a monoclinic crystal of hen egg-white lysozyme (HEWL), we visualized the attachment and detachment processes of individual fluorescent-labeled HEWL (F-HEWL) molecules by a fluorescent single-molecule visualization technique. We measured the changes in number density of F-HEWL molecules, whose positions were not changed for longer than a certain residence time, as a function of an adsorption time. We first confirmed that under an equilibrium condition, there was an "induction period" (∼120 min) of the attachment/detachment processes, during which period the number density remained constant. After the induction period, the number density increased linearly with the adsorption time, as it was recently found on a tetragonal HEWL crystal [Dai, G. L. Cryst. Growth Des 2011, 11(1), 88−92]. In addition, we performed similar measurements under a supersaturated condition. Then we found that supersaturation significantly enhanced the attachment process after the induction time. The attachment/detachment processes finally reached a steady state, in which the attachment rate was higher than the detachment one. Moreover, we also found that in a rare case, an F-HEWL molecule adsorbed on a step laterally moved following the advancement of a growing step.

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Elementary steps at the surface of ice crystals visualized by advanced optical microscopy

Cited by 110 publications

References 46 publications

Quasi-liquid layers on ice crystal surfaces are made up of two different phases

Quasi-liquid layers on ice crystal surfaces are made up of two different phases

Ultraslow growth rates of giant gypsum crystals

Attachment and Detachment Processes of Individual Lysozyme Molecules on a Surface of a Monoclinic Lysozyme Crystal Studied by Fluorescent Single-Molecule Visualization

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