Observations of snow crystals using low-temperature scanning electron microscopy

Low-temperature scanning electron microscopy (SEM) was used to observe precipitation particles commonly known as “snowflakes.” The snowflakes were collected in Beltsville, Maryland, at temperatures ranging from ?6° to +1°C, mounted on SEM stubs, frozen in liquid nitrogen (LN₂), and then transferred to a cryosystem mounted on a field-emission SEM. Neither sputter coating with platinum nor irradiation by the electron beam affected their delicate fine structure. SEM observations revealed that snowflakes consisted of aggregations of snow crystals that occurred as hexagonal plates, prismatic columns, needles, and dendrites. In some cases, the snow crystals contained minute surface structures that consisted of rime, microdroplets, short prismatic columns, and amorphous films. Snow crystals from wet snow, which were collected at temperatures of 0° and +1°C, exhibited varying degrees of metamorphism or melting. The discrete crystalline faces and their sharp intersecting angles were gradually replaced by sinuous surfaces that tended to exhibit more spherical shapes. This study indicates that low-temperature SEM is a valuable technique for studying the formation and metamorphosis of snow crystals. The results suggest that combining low-temperature SEM and x-ray analysis could also provide qualitative elemental information on the nucleation particles of snow crystals as well as on the composition of acid snow.     

Use of low-temperature scanning electron microscopy to compare and characterize three classes of snow cover

This study, which uses low-temperature scanning electron microscopy (LTSEM), systematically sampled and characterized snow crystals that were collected from three unique classes of snow cover: prairie, taiga, and alpine. These classes, which were defined in previous field studies, result from exposure to unique climatic variables relating to wind, precipitation, and air temperature. Snow samples were taken at 10 cm depth intervals from the walls of freshly excavated snow pits. The depth of the snow pits for the prairie, taiga, and alpine covers were 28, 81, and 110 cm, respectively. Visual examination revealed that the prairie snow cover consisted of two distinct layers whereas the taiga and alpine covers had four distinct layers. Visual measurements were able to establish the range of crystal sizes that occurred in each layer, the temperature within the pit, and the snow density. The LTSEM observations revealed the detailed structures of the types of crystals that occurred in the snow covers, and documented the metamorphosis that transpired in the descending layers. Briefly, the top layers from two of the snow covers consisted of freshly fallen snow crystals that could be readily distinguished as plates and columns (prairie) or graupel (taiga). Alternatively, the top layer in the alpine cover consisted of older dendritic crystal fragments that had undergone early metamorphosis, that is, they had lost their sharp edges and had begun to show signs of joining or bonding with neighboring crystals. A unique layer, known as sun crust, was found in the prairie snow cover; however, successive samplings from all three snow covers showed similar stages of metamorphism that led to the formation of depth hoar crystals. These changes included the gradual development of large, three-dimensional crystals having clearly defined flat faces, sharp edges, internal depressions, and facets. The study, which indicates that LTSEM can be used to enhance visual data by systematically characterizing snow crystals that are collected at remote locations, is important for understanding the physics of snowpacks and the metamorphosis that leads to potential avalanche situations. In addition, the metamorphosis of snow crystals must be considered when microwave radiometry is used to estimate the snow water equivalent in the winter snowpack, because large snow crystals more effectively scatter passive microwave radiation than small crystals.     

Irregular snow crystals: structural features as revealed by low temperature scanning electron microscopy

For nearly 50 years, investigators using light microscopy have vaguely alluded to a unique type of snow crystal that has become known as an irregular snow crystal. However, the limited resolution and depth-of-field of the light microscope has prevented investigators from characterizing these crystals. In this study, a field-emission scanning electron microscope, equipped with a cold stage, was used to document the structural features, physical associations, and atmospheric metamorphosis of irregular snow crystals. The crystals appear as irregular hexagons, measuring 60 to 90 mm across, when viewed from the a-axis. Their length (c-axis) rarely exceeds the diameter. The irregular crystals are occasionally found as secondary particles on other larger forms of snow crystals; however, they most frequently occur in aggregates consisting of more than 100 irregular crystals. In the aggregates, the irregular crystals have their axes oriented parallel to one another and, collectively, tend to form columnar structures. Occasionally, these columnar structures exhibit rounded faces along one side, suggesting atmospheric metamorphoses during formation and descent. In extreme cases of metamorphoses, the aggregates would be difficult to distinguish from graupel. Frost, consisting of irregular crystals, has also been encountered, suggesting that atmospheric conditions that favor their growth can also occur terrestrially.     

Characterization of the annealed (0001) surface of sapphire (alpha-Al2O3) and interaction with silver by reflection electron microscopy and scanning reflection electron microscopy.

Annealed (0001) surfaces of single-crystal sapphire (alpha-Al2O3) rod have been studied in the electron microscope using reflection electron microscopy (REM), scanning reflection electron microscopy (SREM), and reflection high energy electron diffraction (RHEED). Annealed surfaces of (0001) sapphire are vicinal and characterized by close-packed (0001)-oriented terraces separated by faceted multiple-height steps, with edges parallel to energetically preferred low-index directions (less than 1010 greater than and less than 1120 greater than). These structural features are not seen on cleaved surfaces or polished surfaces treated at temperatures less than 1,250 degrees C. Oxygen-annealing produces clean surfaces which prove useful for investigating the interaction of deposited metals with the (0001) sapphire. Both REM and SREM (with microdiffraction spots) techniques have been used to observe fine structure of flat Ag islands on the scale of 1-100 nm on the (0001)-oriented terraces as well as aggregations at the steps. A preliminary result on interaction with Cu is also included.     

Morphological analyses of minute crystals by using stereo-photogrammetric scanning electron microscopy and electron back-scattered diffraction

We present a new method for the morphological analyses of minute faceted crystals by combining stereo-photogrammetric analysis of scanning electron microscope images and electron back-scattered diffraction. Two scanning electron microscope images of the same crystal, recorded at different tilt angles of the specimen stage, are used to determine the orientations of crystal edges in a specimen-fixed coordinate system. The edge orientations are converted to the indices [ uvw ] in the crystal system using the crystal orientation determined by electron back-scattered diffraction analysis. The Miller indices of crystal facets are derived from the indices of the edges surrounding the facets. The method is applicable to very small crystal facets. The angular error, as derived from tests using a calcite crystal of known morphology, is a few degrees.
To demonstrate the applicability of the method, the morphology of boehmite (γ-AlOOH) precipitated from solution during the dissolution of anorthite was analyzed. The micrometre-sized boehmite crystals are surrounded by two {010} basal facets and eight equivalent side facets that can be indexed equally well as {323}, {434} or {545}. We suggest that these side facets are in fact {111}, the morphology having been modified slightly (by a few degrees) by a small extension associated with opening along (010) microcleavage planes. Tiny {140} facets are also commonly observed.     

Image comparisons of snow and ice crystals photographed by light (video) microscopy and low-temperature scanning electron microscopy

Light (video) microscopy and low-temperature scanning electron microscopy (SEM) were used to examine and record images of identical precipitated and metamorphosed snow crystals as well as glacial ice grains. Collection procedures enabled numerous samples from distant locations to be shipped to a laboratory for storage and/or observation. The frozen samples could be imaged with a video microscope in the laboratory at ambient temperatures or with the low-temperature SEM. Stereo images obtained by video microscopy or low-temperature SEM greatly increased the ease of structural interpretations. The preparation procedures that were used for low-temperature SEM did not result in sublimation or melting. However, this technique did provide far greater resolution and depth of focus over that of the video microscope. The advantage of resolution was especially evident when examining the small particles associated with rime and graupel (snow crystals encumbered with frozen water droplets), whereas the greater depth of focus provided clearer photographs of large crystals such as depth hoar, and ice. Because the SEM images contained only surface information while the video images were frequently confounded by surface and internal information, the SEM images also clarified the structural features of depth hoar crystals and ice grains. Low-temperature SEM appears to have considerable promise for future investigations of snow and ice.     

Irregular Helium Bubbles In Niobium Alloys

Helium bubbles have been produced in niobium-1% Zr by ion implantation and their growth has been studied by transmission electron microscopy of annealed specimens. Bubbles are normally faceted and develop from tetrakaidodecahedra at short times to cuboids bounded by {100} faces after long annealing periods. This behaviour, together with the observation of steps on the faces of many bubbles, is accounted for in terms of competition between the conditions necessary for thermodynamic equilibrium and the kinetics of bubble motion. The larger bubbles must contain an excess gas pressure.     

Multi-scale simulations of field ion microscopy images--image compression with and without the tip shank

Multi-scale simulations of field ion microscopy images of faceted and hemispherical samples are performed using a 3D model. It is shown that faceted crystals have compressed images even in cases with no shank. The presence of the shank increases the compression of images of faceted crystals quantitatively in the same way as for hemispherical samples. It is hereby proven that the shank does not influence significantly the local, relative variations of the magnification caused by the atomic-scale structure of the sample.     

Cryogenic EBSD on ice: preserving a stable surface in a low pressure SEM

Naturally deformed ice contains subgrains with characteristic geometries that have recently been identified in etched surfaces using high-resolution light microscopy (LM). The probable slip systems responsible for these subgrain boundary types can be determined using electron backscattered diffraction (EBSD), providing the etch features imaged with reflected LM can be retained during EBSD data acquisition in a scanning electron microscope (SEM). Retention of the etch features requires that the ice surface is stable. Depending on the pressure and temperature, sublimation of ice can occur. The equilibrium temperature for a low pressure SEM operating at 1 × 10(-6) hPa is about -112°C and operating at higher temperatures causes sublimation. Although charging of uncoated ice samples is reduced by sublimation, important information contained in the etch features are removed as the surface sublimes. We developed a method for collecting EBSD data on stable ice surfaces in a low pressure SEM. We found that operating at temperatures of <-112°C reduced sublimation so that the original etch surface features were retained. Charging, which occurred at low pressures (<1.5 × 10(-6) to 2.8 × 10(-5) hPa) was reduced by defocusing the beam. At very low pressures (<1.5 × 10(-6) hPa) the spatial resolution with a defocused beam at 10 kV was about 3 μm in the x-direction at -150°C and 0.5 μm at -120°C, because at higher temperature charging was less and only a small defocus was needed to compensate it. Angular resolution was better than 0.7° after orientation averaging. Excellent agreement was obtained between LM etch features and EBSD mapped microstructures. First results are shown, which indicate subgrain boundary types comprised of basal (tilt and twist) and nonbasal dislocations (tilt boundaries).     

疲劳近门槛值区裂纹扩展模式变化的试验研究

利用扫描电镜观察疲劳门槛值区试样的裂纹表面形貌,研究了疲劳门槛值区裂纹扩展模式的分布,分析了裂纹扩展模式的变化对疲劳裂纹扩展速率da／dN的影响。结果表明,断口形貌存在面型断裂（沿晶或穿晶）（Faceted Fracture,FF）,面型断裂分数（Percentageof Faceted Fracture,PFF）最大值出现在循环塑性区尺寸接近原始奥氏体晶粒直径时。通过比较循环塑性区尺寸与晶粒尺寸,随着应力强度因子幅值AK的降低,裂纹先以辉纹型模式扩展,在PFF达到最大值后,裂纹以晶体学模式扩展。辉纹型模式扩展时,PFF的变化对da／dN影响不大;晶体学模式扩展时,由于FF诱发裂纹闭合,从而降低da／dN。     

Nanoscale TiO island formation on the SrTiO3(001) surface studied by in situ high-resolution transmission electron microscopy

The formation and time evolution of TiO islands on SrTiO3(001) surface facets at 970 degrees C are studied by in situ high-resolution transmission electron microscopy (HRTEM). The exact surface morphology of the islands and the interface between the islands and the SrTiO3 bulk are characterized by profile imaging in cross-section. At the initial stage of formation, the islands contain crystal defects which disappear after annealing times for longer than 100 min. Lattice parameter measurement from the HRTEM images reveals that the crystal islands may be identified as TiO. They are faceted in shape, having the {001} and {011} facet components. During annealing for about 2.5 h the islands grow to sizes of 3-4 nm in equivalent sphere radius, and shrink again during longer annealing. The interface between the TiO islands and the SrTiO3 bulk also shows faceting.     

In situ dynamic HR-TEM and EELS study on phase transitions of Ge2Sb2Te5 chalcogenides

The phase transition phenomena of Ge2Sb2Te5 chalcogenides were investigated by in situ dynamic high-resolution transmission electron microscopy (HR-TEM) and electron energy loss spectroscopy (EELS). A 300kV field emission TEM and a 1250kV high voltage TEM were employed for the in situ heating experiments from 20 to 500 degrees C for undoped and 3wt% nitrogen-doped Ge2Sb2Te5 thin films deposited by DC sputtering. Crystallization of amorphous Ge2Sb2Te5 to its cubic structure phase started at 130 degrees C and then rapid crystal growth developed from cubic to hexagonal phase in the range of 130-350 degrees C; finally, the hexagonal crystals started to melt at 500 degrees C. For nitrogen-doped Ge2Sb2Te5, its crystallization from amorphous film occurred at higher temperature of ca. 200 degrees C, and the cubic and hexagonal phases were usually formed simultaneously without significant growth of crystals at further heating to 400 degrees C. EELS measurements showed that the electronic structures of Ge, Sb and Te stayed almost the same regardless of the amorphous, FCC and hexagonal phases. The nitrogen doped in Ge2Sb2Te5 was confirmed to exist as a nitride. Also, the doped nitrogen distributed homogeneously in both amorphous and crystalline phases. Localization of doped nitrogen was not found in the grain boundary of crystallized phases. The dynamic process of phase transition was enhanced by high-energy electron irradiation. Peeling of atomic layers in nitrogen-doped Ge2Sb2Te5 film was detected during heating assisted with electron beam irradiation.     

New growth features of natural diamonds,revealed by color cathodoluminescence scanning electron microscope (CCL SEM) technique

The internal structure of diamonds with various habit was studied by color cathodoluminescence scanning electron microscopy (CCL SEM). A new growth mechanism was ascertained for diamonds of rounded and octahedral habit. The specific growth details found by means of CCL SEM testify to the fact that the crystallization of diamonds proceeded from the specimen periphery toward the centre by formation of agate secretions. CCL determined was the structure of transparent cubic crystals to be a combination of zones with cuboid surfaces and fibrous structure. The authors consider that both cuboid and fibrous structures are the result of normal (nontangential) growth mechanisms which may be realized during secretional filling of the space, determined for a number of crystals of rounded and octahedral habitus.     

Algebraic model of turbulent flow in ducts of rectangular cross-section with rounded corners

Of increasing importance are nowadays ducts of rectangular cross-section with large-radius rounded corners. They are used for large air flow rates at low pressure levels — typically for air flow distribution in buildings ventilation and heating systems. Paper develops an analytic model of turbulent flows in these ducts. It makes possible in particular evaluation of velocity profiles – and volume flow rates as a function of duct cross-section shapes. The model was validated by comparing the solutions with full-scale duct laboratory measurements.     

A Sublimation Silicon Molecular-Beam Epitaxy System

An ultrahigh-vacuum system with sublimation sources of silicon vapors is described. Two sublimation silicon sources in the form of 90-mm-long rods with a cross section of 4 × 4 mm²were used in the procedure of growing high-quality silicon layers. The rods were cut out from ingots of pure Si single crystals or from preliminarily doped crystals with various types of conductivities. The holders of the sources contained no metallic parts in direct contact with silicon heated up to 1380°C. The sources were heated by the current passed through them and were multiply evaporated onto the substrate. A typical growth rate is 1.5 m/h at 3-cm distance between source and substrate.The pressure in the growth chamber during evaporation was maintained close to the basic one (<1 × 10^–8Torr). Photoluminescence measurements of the grown silicon layers showed their perfect crystalline quality.     

Protrusion recognition from solid model using orthogonal bounding factor

Feature recognition is important for describing shapes in many applications taking advantage of solid modeling. Graph-based feature recognition methods search from solid models the unique patterns of features that are represented as a graph. A typical example of such patterns is a loop of concave edges. When the loop is an inner loop on a single face, it is a strong hint of the existence of protrusion feature and recognition of protrusion faces is straightforward. However, when a protrusion feature lies on multiple faces, it is bounded by a loop of concave edges that are not on a single face. Consequently, the rule of inner loop is no more available and recognition of protrusion faces becomes unclear. To address this problem, a new quantitative measure, orthogonal bounding factor (OBF), is introduced. OBF is defined as the sum of cross products of two consecutive vectors normal to a set of faces, and it physically represents the possibility of being a protrusion in a solid model. The formal definition of orthogonal bounding factor is established and a method to recognize protrusion features using OBF is presented. Examples are also shown to demonstrate the effectiveness of the method for feature recognition.     

A freeze-fracture replication apparatus for biological specimens.

A freeze-fracture apparatus of original design has been constructed which can be fitted onto a standard vacuum evaporator unit. In it, cell suspensions and organized tissue may be processed by inserting a sample into a cylindrical holder. By leaving a small part of the tissue protruding from the holder, pre-selected and aligned portions of the specimen can subsequently be revealed by fracture under vacuum. After rapid freezing, the specimen remains firmly attached to the inner wall of the sample holder, preventing its possible loss during fracturing. A mechanism, in the form of a double-sided converging wedge, which is operated from outside the vacuum chamber, is used to produce a fracture in the specimen. The device gently induces a fracture in the desired part of the tissue and lifts the protruding part of the specimen out of the way. In this way, reasonably flat fracture faces are produced for subsequent replication. As the fracturing mechanism comes into contact only with the outer edges of the specimen, damage and contamination liable to occur when the entire specimen is traversed by a blade, is avoided. In addition the specimen stage is surrounded by a cold metal shroud which acts as an efficient trap for contaminants. In this way, favourable vacuum conditions are produced in the vicinity of the specimen. Such effective enclosing of the specimen also facilitates controlled sublimation of the sample.     

High-load, high-temperature deformation apparatus for synthetic and natural silicate melts

A unique high-load, high-temperature uniaxial press was developed to measure the rheology of silicate melts and magmatic suspensions at temperature up to 1050 degrees C. This new apparatus is designed to operate at constant stresses (up to 300 kN) or constant strain rates (approximately 10(-7) to 10(0) s(-1)) and further allows us to carry on experiments on samples with high viscosities (approximately 10(8) to 10(12) Pa s). The rheological instrument represents an advance in that it accommodates homogeneously heated samples (+/-2 degrees C) of voluminous sizes (up to 790 cm(3)) which permit the insertion of thermocouples to monitor temperature distribution evolutions during measurements. At last this setup allows for accurate measurements of viscosity of natural multiphase materials at strain rates and temperatures common to natural systems. The apparatus aspires to precisely (1) describe the onset of non-Newtonian behavior and its evolution with increasing strain rate until the point of rupture in the brittle regime, (2) constrain the effect of crystals and bubbles on the viscosity, and (3) record heating dissipated through viscous deformation. Here, we present a series of measurements on NIST standard material SRM 717a to calibrate the instrument. We couple the viscosity determined via Gent's equation with certified viscosity data of the standard material to calibrate this state-of-the-art apparatus. This work shows that we can resolve the viscosity of voluminous melt sample within 0.06 logarithmic unit and furthermore present the detection of minor viscous dissipation for a high-temperature, high strain rate experiment.