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We present evidence that in ~ 1650 BCE (~ 3600 years ago), a cosmic airburst destroyed Tall el-Hammam, a Middle-Bronze-Age city in the southern Jordan Valley northeast of the Dead Sea. The proposed airburst was larger than the 1908 explosion over Tunguska, Russia, where a ~ 50-m-wide bolide detonated with ~ 1000× more energy than the Hiroshima atomic bomb. A city-wide ~ 1.5-m-thick carbon-and-ash-rich destruction layer contains peak concentrations of shocked quartz (~ 5–10 GPa); melted pottery and mudbricks; diamond-like carbon; soot; Fe- and Si-rich spherules; CaCO3 spherules from melted plaster; and melted platinum, iridium, nickel, gold, silver, zircon, chromite, and quartz. Heating experiments indicate temperatures exceeded 2000 °C. Amid city-side devastation, the airburst demolished 12+ m of the 4-to-5-story palace complex and the massive 4-m-thick mudbrick rampart, while causing extreme disarticulation and skeletal fragmentation in nearby humans. An airburst-related influx of salt (~ 4 wt.%) produced hypersalinity, inhibited agriculture, and caused a ~ 300–600-year-long abandonment of ~ 120 regional settlements within a > 25-km radius. Tall el-Hammam may be the second oldest city/town destroyed by a cosmic airburst/impact, after Abu Hureyra, Syria, and possibly the earliest site with an oral tradition that was written down (Genesis). Tunguska-scale airbursts can devastate entire cities/regions and thus, pose a severe modern-day hazard.

Multi-proxy analyses of a sequence spanning the Younger Dryas (YD) in the Glacial Lake Hind basin of Manitoba provides insight into regional paleohydrology and paleovegetation of meltwater rivers and lakes spanning >4000 yr; the sequence is controlled by 25 new accelerator mass spectrometry ages. This lake, dammed by the Laurentide Ice Sheet, overflowed into Lake Agassiz. The pre-YD interval records rapid sedimentation from meltwaters that headed in proglacial lakes in the Canadian Prairies that are known to have been catastrophically released when ice or sediment barriers were breached. Pollen in this phase is dominated by pre-Quaternary forms eroded from Paleocene bedrock. At the onset of the YD at ~12.8 cal ka, the sudden appearance of concentrations of nanodiamonds, high-temperature magnetic spherules, platinum, and iridium provide evidence of an extraterrestrial (ET) event that others have identified at more than 40 sites in North America. Major changes in oceans and climate, and the catastrophic outflow of nearby Lake Agassiz at the onset of the YD, may be related. Lower water levels and a reduction of Souris River inflow to Lake Hind followed, which are reflected by more clayey and organic-rich sediments and a decrease in pre-Quaternary palynomorphs. This may have resulted from the deepening of river valleys caused by the release of meltwater triggered by the ET event. Wetlands then began to develop, leading to peat deposition from 12.3 to 11 cal ka. This was followed by a fluvial episode depositing sand and then by increased Holocene aridity that resulted in accumulation of a thick sequence of dune sands. A dry woodland environment with a mix of conifers (especially Picea and Larix) and deciduous trees (especially Populus and Quercus) covered the uplands from ~13 to 10 cal ka.

The Younger Dryas (YD) impact hypothesis posits that fragments of a large, disintegrating asteroid/comet struck North America, South America, Europe, and western Asia ~12,800 years ago. Multiple airbursts/impacts produced the YD boundary layer (YDB), depositing peak concentrations of platinum, high-temperature spherules, meltglass, and nanodiamonds, forming an isochronous datum at >50 sites across ~50 million km² of Earth’s surface. This proposed event triggered extensive biomass burning, brief impact winter, YD climate change, and contributed to extinctions of late Pleistocene megafauna. In the most extensive investigation south of the equator, we report on a ~12,800-year-old sequence at Pilauco, Chile (~40°S), that exhibits peak YD boundary concentrations of platinum, gold, high-temperature iron- and chromium-rich spherules, and native iron particles rarely found in nature. A major peak in charcoal abundance marks an intense biomass-burning episode, synchronous with dramatic changes in vegetation, including a high-disturbance regime, seasonality in precipitation, and warmer conditions. This is anti-phased with northern-hemispheric cooling at the YD onset, whose rapidity suggests atmospheric linkage. The sudden disappearance of megafaunal remains and dung fungi in the YDB layer at Pilauco correlates with megafaunal extinctions across the Americas. The Pilauco record appears consistent with YDB impact evidence found at sites on four continents.

Biocoatings concentrate living, nongrowing microbes in nanoporous adhesive polymer films. Any microbial activity or trait of interest can be intensified and stabilized in biocoatings. These films will dramatically expand the functionality of waterborne coatings. Many microbes contain enzyme systems which are unstable when purified. Therefore, thin polymer coatings of active microbes are a revolutionary approach to stabilize living cells as industrial or environmental biocatalysts. We have demonstrated that some microbes survive polymer film formation embedded in nontoxic adhesive waterborne binders by controlling formulation and drying. Biocoatings can be a single layer of randomly oriented microbes or highly structured multilayer films combining monolayers of different types of microbes on solid, porous, or flexible substrates. They can be formed by drawdown or ink-jet deposition, convective sedimentation assembly, dielectrophoresis, or coated onto or embedded within papers. Controlled drying generates nanoporous microstructure; the pores are filled with a carbohydrate glass which stabilizes the entrapped dehydrated microbes. When the coating is rehydrated, the carbohydrates diffuse out generating nanopores. The activity of biocoatings can be 100s of g L−1 (coating volume) h−1 stabilized for 100–1000s of hours, and therefore, they represent a new approach to process intensification (PI) using thin liquid film bioreactors. A current challenge is that many microbes being engineered as environmental, solar, or carbon recycling biocatalysts do not naturally survive film formation. The mechanisms of dehydration damage that occur during biocoating formulation, ambient drying, and during dry storage have begun to be studied. Critical to preserving microbe viability are minimizing osmotic stress, toxic monomers, biocides, and utilizing polymer chemistries that generate strong wet adhesion with arrested coalescence (nanoporosity). Therefore, controlling desiccation, drying rate/uniformity, and residual moisture are important. Optimization of biocoating activity can be affected at multiple stages—cellular engineering prior to coating (preadaptation), formulation, deposition (film thickness), film formation/drying (generates microstructure), dry storage (minimize metabolic activity), and rehydration. Gene induction (activation) leading to enzyme synthesis following rehydration has been demonstrated. However, little is known about gene regulation in nongrowing microbes. Challenges to optimizing biocoating activity include generating stable film porosity, strong wet adhesion, control of residual water content/form/distribution, and nondestructive measurement of entrapped microbe viability and activity. Indirect methods to measure viability include vital staining, enzyme activity, reporter genes, response to light, confocal fluorescent microscopy, and ATP content. Microbes containing stress-inducible reporter genes can be used to monitor cell stress during formulation, film formation, and drying. Future cellular engineering to optimize biocoatings includes desiccation tolerance, light reactivity (photoefficiency), response to oxidative stress, and cell surface-to-polymer or substrate adhesion. Preservation of microbial activity in waterborne coatings could lead to high intensity biocatalysts for environmental cleaning, gaseous carbon recycling, to produce H2 or electricity from microbial fuel cells, delivery of probiotics, or for biosolar energy harvesting.

We propose a novel approach to continuous bioprocessing of gases. A miniaturized, coated-paper strip, high gas fraction, biocomposite absorber has been developed using slowly shaken horizontal anaerobic tubes. Concentrated Clostridium ljungdahlii OTA1 was used as a model system. These gas absorbers demonstrate elevated CO mass transfer with low power input, reduced liquid requirements, elevated substrate consumption, and increased product secretion compared to shaken suspended cells. Concentrated OTA1 cell paste was coated by extrusion onto chromatography paper. The immobilized system shows high, constant reactivity immediately upon rehydration. Cell adhesion was by adsorption to the cellulose fibers; visualized by SEM. The C. ljungdahlii OTA1 coated paper mounted above the liquid level absorbs CO and H2 from a model syngas secreting acetate with minimal ethanol. At 100 rpm shaking speed (7.7 Wm(-3) ) the optimal cell loading is 6.5 gDCW m(-2) to maintain high CO absorbing reactivity without the cells coming off of the paper into the liquid phase. Reducing the medium volume from 10 mL to 4 mL (15% of tube volume) did not decrease CO reactivity. The reduced liquid volume increased secreted product concentration by 80%. The specific CO consumption by paper biocomposites was higher at all shaking frequencies

A major impediment to the widespread use of asphalt concrete with a high content of reclaimed asphalt pavement (RAP) is uncertainty in the degree of blending between the RAP and the fresh binder. Furthering knowledge concerning the blending between RAP and fresh binder has been difficult because of the lack of an experimental method to quantify the degree of blending in asphalt concrete. This study introduces energy dispersive X-ray spectroscopy (EDS) scanning electron microscopy (SEM) as a means to analyze the degree of blending between RAP and fresh materials in asphalt concrete. EDS allows for mapping the distribution and relative proportion of elements in a sample, hence, allowing for the detection of the distribution of elements in an asphalt concrete specimen. Fresh and RAP binders will have a similar elemental composition. Therefore, titanium dioxide in a fine powder form (0.15-µm particles) is blended with the fresh binder as a tracer before the production of asphalt concrete to enable delineation of the RAP and fresh binders using EDS SEM. The efficacy of EDS SEM for quantifying the degree of blending between RAP and fresh binders in asphalt concrete is demonstrated with two high RAP content mixtures.

We describe a latex wet coalescence extrusive coating method that produces up to 10-fold specific photosynthetic rate enhancements by nitrate-limited non-growing cyanobacteria deposited onto paper, hydrated and placed in the gas-phase of small tube photobioreactors. These plant leaf-like biocomposites were used to study the tolerance of cyanobacteria strains to illumination and temperature using a solar simulator. We report sustained CO2 absorption and O2 production for 500 h by hydrated gas-phase paper coatings of non-growing Synechococcus PCC7002, Synechocystis PCC6803, Synechocystis PCC6308, and Anabaena PCC7120. Nitrate-starved cyanobacteria immobilized on the paper surface by the latex binder did not grow out of the coatings into the bulk liquid. The average CO2 consumption rate in Synechococcus coatings is 5.67 mmol m−2 h−1 which is remarkably close to the rate reported in the literature for Arabidopsis thaliana leaves under similar experimental conditions (18 mmol m−2 h−1). We observed average ratios of oxygen production to carbon dioxide consumption (photosynthetic quotient, PQ) between 1.3 and 1.4, which may indicate a strong dependence on nitrate assimilation during growth and was used to develop a non-growth media formulation for intrinsic kinetics studies. Photosynthetic intensification factors (PIF) (O2 production by nitrate-limited cyanobacteria in latex coatings/O2 produced by nitrate-limited cell suspensions) in cyanobacteria biocomposites prepared from wet cell pellets concentrated 100- to 300-fold show 7–10 times higher specific reactivity compared to cells in suspension under identical nitrate-limited non-growth conditions. This is the first report of changes of cyanobacteria tolerance to temperature and light intensities after deposition as a thin coating on a porous matrix, which has important implications for gas-phase photobioreactor design using porous composite materials. Cryo-fracture SEM and confocal microscopy images of cell coating distribution on the paper biocomposite suggest that the spatial arrangement of the cells in the coating can affect photoreactivity. This technique could be used to fabricate very stable, multi-organism composite coatings on flexible microfluidic devices in the gas-phase capable of harvesting light in a broader range of wavelengths, to optimize thermotolerant, desiccation tolerant, or halotolerant cyanobacteria that produce O2 with secretion of liquid-fuel precursors synthesized from CO2. Biotechnol. Bioeng. 2014;111: 1993–2008. © 2014 Wiley Periodicals, Inc.

Quantitative characterization of a diamond tool profile is critical to reveal tool wear mechanisms. An electron-beam-induced deposition (EBID) method reported previously is further developed and improved to measure diamond tool profiles using a field emission scanning electron microscope (SEM). The edge radius and wear land length for new and worn diamond tools were derived from analysis of the EBID-SEM images. Experimental results are presented to show that the methodology is an effective means to characterize diamond tool wear.

A high-vacuum low-temperature atomic force microscope (AFM) for the direct observation of freeze-fracture samples has been developed. This AFM has a freeze-fracture mechanism inside the vacuum chamber. With this AFM it is possible to observe the fractured surface directly without both fabricating a replica and exposure to the ambient atmosphere. Both sandwich and knife fracture methods have been achieved to obtain freeze-fracture surfaces and after deep etching. A fine structure of the fractured red blood cell membrane has been observed using both methods. These are relatively quick and easy methods for the observation of freeze-fracture surfaces without introducing replica artifacts.

The North American river otter (Lontra canadensis) serves as an indicator species for environmental monitoring, is prized as a valuable furbearer, and is a popular display animal in zoologic collections. Nephrolithiasis has been reported as a frequent problem in other free-ranging and captive otter species but is rarely reported in North American river otters. In this study, we compared the prevalence of nephrolithiasis diagnosed using routine gross pathologic examination techniques with the use of computed tomography (CT) of excised kidneys. We also evaluated whether otter nephroliths could be accurately classified by their CT densities, and we examined the renal tissue uric acid concentrations in free-ranging otters in North Carolina, USA. Kidneys were collected from carcasses of legally trapped, free-ranging animals. Nephroliths were observed in 16.2% of the individuals (n ¼ 229). Associations were found between age and nephrolith status and between capture location and nephrolith status (P ¼ 0.026 and , 0.001, respectively). Computed tomography Hounsfield unit density measurements were not useful in determining nephrolith chemical composition in this study. Renal tissue uric acid concentrations were similar across genders, age groups, and stone status. The chemical composition of the nephroliths was determined by scanning electron microscopy-energy dispersive X-ray spectroscopy to be calcium phosphate in the carbonate form.

The results of contact potential difference (CPD) imaging on Au-deposited p-type and n-type Si(111) 7×7 surfaces are discussed. The scanning Kelvin probe microscopy (SKPM) technique based on the gradient of the electrostatic force was used under ultrahigh vacuum (UHV) conditions to acquire the data presented. The CPD images of Au deposited on the Si(111) 7×7 surface show virtually identical features, irrespective of whether the Si is n- or p-type. In these images, it is believed that the atomically resolved potential difference does not originate from the intrinsic work function of the materials but reflects the local electron density on the surface. On the other hand, the average potentials corresponding to the DC levels in each CPD image reflects the work function value on the surface. The work function of p-type Si(111) 7×7 is found to be higher than that of n-type by about 0.45 eV, where both samples had the same resistivity of about 0.5 Ω cm and the same Au coverage. If the Au coverage is increased, the work function increases.

In PNAS, M. Boslough (1) raises issues about carbon spherules and nanodiamonds unrelated to our magnetic spherule focused research (2). Boslough should instead address the questions he raises to the appropriate investigators.

Firestone et al. sampled sedimentary sequences at many sites across North America, Europe, and Asia [Firestone RB, et al. (2007) Proc Natl Acad Sci USA 106:16016–16021]. In sediments dated to the Younger Dryas onset or Boundary (YDB) approximately 12,900 calendar years ago, Firestone et al. reported discovery of markers, including nanodiamonds, aciniform soot, high-temperature melt-glass, and magnetic microspherules attributed to cosmic impacts/airbursts. The microspherules were explained as either cosmic material ablation or terrestrial ejecta from a hypothesized North American impact that initiated the abrupt Younger Dryas cooling, contributed to megafaunal extinctions, and triggered human cultural shifts and population declines. A number of independent groups have confirmed the presence of YDB spherules, but two have not. One of them [Surovell TA, et al. (2009) Proc Natl Acad Sci USA 104:18155–18158] collected and analyzed samples from seven YDB sites, purportedly using the same protocol as Firestone et al., but did not find a single spherule in YDB sediments at two previously reported sites. To examine this discrepancy, we conducted an independent blind investigation of two sites common to both studies, and a third site investigated only by Surovell et al. We found abundant YDB microspherules at all three widely separated sites consistent with the results of Firestone et al. and conclude that the analytical protocol employed by Surovell et al. deviated significantly from that of Firestone et al. Morphological and geochemical analyses of YDB spherules suggest they are not cosmic, volcanic, authigenic, or anthropogenic in origin. Instead, they appear to have formed from abrupt melting and quenching of terrestrial materials.

Freeze‐fractured human Red Blood Cell (RBC) has been observed directly with a high‐vacuum low‐temperature atomic force microscope (AFM). This AFM has an integrated vacuum evacuation system and a freeze‐fracture mechanism inside the vacuum chamber. The AFM is able to observe the fractured RBC surface without exposure to the ambient atmosphere. With this AFM it is possible to observe the fractured surface directly without fabricating a replica. Both sandwich and knife fracture techniques have been used to obtain freeze fracture surfaces and, after deep etching, fine structure of the RBC membrane has been observed using both methods. The membrane bi‐layer structure is clearly different from membrane surface structure. These are relatively quick and easy methods for the observation of freeze fracture surfaces without introducing replica artifacts.

Extended abstract of a paper presented at Microscopy and Microanalysis 2006 in Chicago, Illinois, USA, July 30 – August 3, 2005

Extended abstract of a paper presented at Microscopy and Microanalysis 2004 in Savannah, Georgia, USA, August 1–5, 2004.

In recent years, the magnetic force microscope (MFM) has been used not only for the evaluation of magnetic media but also for the measurement of magnetic characteristics of quantum dots as well as in various fields, because the MFM can visualize magnetic field on the sample surface with the high resolution. The MFM observation in ultra-high vacuum (UHV) requires to reduce the adsorption layer on the sample surface for high resolution observation. The slope detection mode using the variation of vibrating cantilever is basically unstable in UHV due to the increase in the Q factor of the cantilever. Accordingly it has been used for the MFM observation in air. On the other hand, the FM detection technique offers a very high sensitivity because of the high Q factor.This repot describes the MFM technique to take a magnetic image steadily in UHV. We observed the surface of a magnetic material with MFM technique in UHV, and compared the slope detection technique, the phase detection technique using phase variation of cantilever vibration, and the FM detection technique.

The scanning Kelvin probe force microscope (SKPM) is a member of the scanning probe microscope (SPM) family, and was derived from the non-contact atomic force microscope (NCAFM) technique. The contact potential difference (CPD) originating from the work function difference between the tip and sample surfaces can be measured using SKPM with simultaneous observation of the topography image. Using SKPM the surface of semiconductor device has been observed to measure the dopant concentration as the CPD difference in two dimensions. Most of the SKPM measurements are acquired in the atmosphere. The lateral resolution is achieved less than 100 nm.On the other hand, Scanning capacitance microscope (SCM) of contact mode is now most popular method to measure the dopant concentration in semiconductor device. However, the lateral resolution of SCM is limited, because of the fact that the contact mode cannot achieve a true atomic resolution, the fact that the capacitance is measured through the insulating layer on surface, and the fact that the tip and sample is damaged by the high electric field to be applied between the tip and sample. So SCM never achieves the atomic level resolution.

We have measured cantilever resonance frequency versus sample bias voltage and generated frequency vs bias ( f–V) curves using an ultrahigh-vacuum noncontact atomic force microscope (UHV NC-AFM). Using the f–V data, we calculated the contact potential difference (CPD) between the tip and the sample. These CPD measurements were compared with those that were directly observed with a scanning Kelvin probe force microscope (SKPM) on the same atomically resolved area of the sample using a UHV-AFM. The CPD values obtained by both methods were similar, however, it was difficult to obtain CPD values that agreed precisely on the atomic scale.

A scanning near-field optical microscope (SNOM) with a nanometer-size aperture cantilever is a new powerful tool for investigating the optical characteristics of specimen surfaces. We applied the AC-mode feedback and gate pulse acquisition methods in illumination/reflection-mode SNOM. The application of the AC-mode feedback method increased the optical intensity of reflected light from two-to seven fold that obtained by the contact-mode feedback method. The use of the gate pulse acquisition method reduced optical imaging artifacts originating from the topographical features of surfaces.

When imaging with an Atomic-Force Microscope (AFM), the image resolution is a complex function of the relative tip and sample geometries. When imaging or measuring high aspect ratio features, sharp and slender tips offer the possibility of probing down into extremely small topographical features. The most commonly used contact mode AFM tips are thin film cantilevers of Si3N4 with an integrated pyramidal structure used as the tip. It has been shown that microtips, which are fabricated by electron beam induced growth of carbonaceous material on the apex of the pyramid, can reduce the artifacts associated with integrated pyramidal AFM tips. A SEM micrograph of a microtip grown on the apex of an integrated pyramid is shown in Figure 1. Use of grown microtips in metrology demands an understanding of the dynamics of microtip deformation while scanning.

Applications of atomic force microscopy (AFM) for the characterization and metrology of technologically-important objects (e.g. x-ray lithography masks) has led to the development of special-purpose, high-aspect-ratio probes. Measuring objects that have deep, narrow trenches requires a controlled probe geometry. The probe radius and aspect ratio determine the congruence of the acquired AFM image to the true profile of the sample. As is illustrated schematically in Figure 1(a), the usual batch-fabricated AFM probe cannot reach down into deep or narrow trenches. Highaspect- ratio AFM probes that can overcome this limitation (Figure lb), have been developed. Probes of ≤100 nm shaft diameter, and up to microns in length, can be grown by electron-beam contamination writing. Focused ion beams have also been used to sharpen conventional probes by rastering a circular pattern around the highest point, removing the“shoulders” by sputtering, and thereby improving the aspect ratio. Previous work has demonstrated the use of such probes in standard, contact-mode AFM. This paper extends the application of these techniques to the creation of probes for resonance-mode AFM, and characterizes the performance of the resulting probes.

The atomic force microscope (AFM) has been used to characterize a variety of surfaces to study the influence of the instrumental parameters and sample topography on the interpretation of the images and the data obtained. The effect of the tip shape on the resulting image resolution and artifacts has been studied. Test samples of varied topography have been used to establish imaging parameter optimization for specific sample topographies.Chromium thin films of different thickness, deposited uniformly by rf diode sputtering, have been selected as test samples and imaged with a variety of tip shapes. These films were developed as underlayer films for magnetic recording media used in computer hard disks. The range of tips include commercial silicon nitride pyramidal tips, focused ion beam (FIB) sharpened silicon nitride pyramidal tips, and electron beam contamination induced tips (microtips) varying in growth time (i.e. length) from 10 to 40 seconds (approximately 0.40 to 0.65 μm).

A high vacuum low temperature atomic force microscope (AFM) for the direct observation of biological freeze–fracture samples has been developed. This AFM has an integrated vacuum system and a freeze–fracture mechanism inside the vacuum chamber. It is possible to observe the fractured sample surface without exposing the freshly fractured surface to the ambient atmosphere. The design is described in detail. A sample temperature up to −175 °C is achieved, with the temperature fluctuation less than 0.1 °C. Temperature control is possible from −175 to 0 °C for deep etching. An ultimate vacuum pressure of 8.7×10−6 Pa has been achieved. Freeze-fractured human red blood cell has been examined, and fine structure within the cell has been observed. It is demonstrated that this is convenient and useful for the direct observation of a biological freeze–fractured surface.

An investigation into improving the tip fabrication technique for Atomic Force Microcopy (AFM) tips has been undertaken. The problems addressed here relate to the artifacts that are produced from imaging high aspect ratio (depth/width) features with standard AFM pyramidal tips. Standard tips, while having a regular geometry present a problem: the pyramid's base is 3-5 microns square and the walls are angled at 55°. This tip shape can cause a great deal of “smoothing” to high aspect ratio topological features, whether they are a few nm or a few μm in height. The use of electron beam grown microtips eliminates many of the tip artifacts found when using standard pyramidal tips. Actual growth of tips is quite easy. Once the SEM is set up properly (focused and stigmated) the scan generator for the beam is turned off, placing the microscope in the spot mode. The beam spot is placed at the point where a tip is desired and left for several minutes.

A low temperature ultrahigh vacuum atomic force microscope (UHV-AFM) has been developed, which allows the sample to be cooled from room temperature to lower than 28 K during observation and can be attached to the conventional UHV-AFM. Atom resolved non-contact atomic force microscopy (NC-AFM) images of the Si(100) surface were obtained at 120 K and 50 K using the produced low temperature UHV-AFM/STM, and the Si(100) dimer structure was successfully observed for the first time by NC-AFM. It was found that the Si(100)-c(4×2) structure mainly covered the area at 120 K, but the p(2×2) structure area increased at 50 K.