Combined micro-Raman Research Articles

Evidence of Correlation between Membrane Phase Transition and Clonogenicity in Dehydrating Acinetobacter baumannii: A Combined Micro-Raman and AFM Study.

The Gram-negative bacterium Acinetobacter baumannii is one of the most resilient multidrug-resistant pathogens in hospitals. Among Gram-negative bacteria, it is particularly resistant to dehydration (anhydrobiosis), and this feature allows A. baumannii to persist in hospital environments for long periods, subjected to unfavorable conditions. We leverage the combination of μ-Raman spectroscopy and atomic force microscopy (AFM) to investigate the anhydrobiotic mechanisms in A. baumannii cells by monitoring the membrane (both inner and outer membranes) properties of four A. baumannii strains during a 16-week dehydration period and in response to temperature excursions. We noted that the membranes of A. baumannii remained intact during the dehydration period despite undergoing a liquid-crystal-to-gel-phase transition, accompanied by changes in the mechanical properties of the membrane. This was evident from the AFM images, which showed the morphology of the bacterial cells alongside modifications of their superficial mechanical properties, and from the alteration in the intensity ratio of μ-Raman features linked to the CH3 and CH2 symmetric stretching modes. Furthermore, employing a universal power law revealed a significant correlation between this ratio and bacterial fitness across all tested strains. Additionally, we subjected dry A. baumannii to a temperature-dependent experiment, the results of which supported the correlation between the Raman ratio and culturability, demonstrating that the phase transition becomes irreversible when A. baumannii cells undergo different temperature cycles. Besides the relevance to the present study, we argue that μ-Raman can be used as a powerful nondestructive tool to assess the health status of bacterial cells based on membrane properties with a relatively high throughput.

A combined micro-Raman, X-ray absorption and magnetic study to follow the glycerol-assisted growth of epsilon-iron oxide sol-gel coatings

Epsilon iron oxide (ε-Fe2O3) coatings on Si(100) substrates are obtained by an easy one-pot sol-gel recipe assisted by glycerol in an acid medium. Glycerol, given its small dimensions, enables the formation of ε-Fe2O3 nanoparticles with a size of a few nanometers and the highest purity is reached in coatings after a densification treatment at 960 °C. The structural and compositional evolution up to 1200 °C is studied by confocal Raman microscopy and X-ray absorption spectroscopy techniques, correlating the existing magnetic properties. We report a novel characterization method, which allows monitoring the evolution of the precursor micelles as well as the intermediate and final phases formed. Furthermore, the inherent industrial technology transfer of the sol-gel process is also demonstrated with the ε-Fe2O3 polymorph, impelling its application in the coatings form.

Near-ultraviolet micro-Raman study of diamond grown on GaN

Ultraviolet (UV) micro-Raman measurements are reported of diamond grown on GaN using chemical vapor deposition. UV excitation permits simultaneous investigation of the diamond (D) and disordered carbon (DC) comprising the polycrystalline layer. From line scans of a cross-section along the diamond growth direction, the DC component of the diamond layer is found to be highest near the GaN-on-diamond interface and diminish with characteristic length scale of ∼3.5 μm. Transmission electron microscopy (TEM) of the diamond near the interface confirms the presence of DC. Combined micro-Raman and TEM are used to develop an optical method for estimating the DC volume fraction.

Complete thermoelectric benchmarking of individual InSb nanowires using combined micro-Raman and electric transport analysis

Nanowires (NWs) are ideal nanostructures for exploring the effects of low dimensionality and thermal conductivity suppression on thermoelectric behavior. However, it is challenging to accurately measure temperature gradients and heat flow in such systems. Here, using a combination of spatially resolved Raman spectroscopy and transport measurements, we determine all the thermoelectric properties of single Se-doped InSb NWs and quantify the figure of merit ZT. The measured laser-induced heating in the NWs and associated electrical response are well described by a 1D heat equation model. Our method allows the determination of the thermal contact resistances at the source and drain electrodes of the NW, which are negligible in our system. The measured thermoelectric parameters of InSb NWs agree well with those obtained based on field-effect transistor Seebeck measurements.

Elemental and spectroscopic characterization of plasters from Fatih Mosque-Istanbul (Turkey) by combined micro-Raman, FTIR and EDXRF techniques

The characterization of the plasters and coloring agents of the wall paintings of Fatih Mosque have been performed using combined micro-Raman, FTIR and EDXRF techniques. The investigations show that the plaster used on the walls has mixed gypsum–lime binders. Cinnabar {HgS}, lead red {Pb3O4} and hematite {α-Fe2O3} were identified in the red surfaces. Blue color is attributed to ultramarine blue {Na8–10Al6Si6O24S2–4}. Green color is assigned to mixtures of green earth, copper phthalocyanine {Cu(C32Cl16N8)} and brochantite {CuSO4·3Cu(OH)2}. Strontium yellow {SrCrO4} and zinc white {ZnO} were also used to ensure the color tone. The results provide a basis for future restoration of wall paints.

A combined microRaman and microdiffraction set-up at the European Synchrotron Radiation Facility ID13 beamline

This article describes the current status of the microRaman set-up at the ID13 beamline of the European Synchrotron Radiation Facility. This offers an in situ on-axis microprobe which has a common focal position to the X-ray microbeam and can collect spectral data simultaneously. It can also be used in an offline sample characterization role, both before and after beamline experiments. To demonstrate the application of microRaman spectroscopy within a beamline environment, a number of examples are given.

Occurrence and distribution of “moganite” in agate/chalcedony: a combined micro-Raman, Rietveld, and cathodoluminescence study

Agate/chalcedony samples of different origin were investigated by performing Raman, X-ray diffraction (using Rietveld refinement), and cathodoluminescence measurements. These analyses were performed to measure the content and spatial distribution of the silica polymorph moganite, which is considered to represent periodic Brazil-law twinning of α-quartz at the unit-cell scale in agate/chalcedonies. Homogeneous standard samples including the nearly α-quartz free moganite type material from Gran Canaria were analysed in order to compare results of the X-ray diffractometry and Raman spectroscopy techniques and to provide a calibration curve for the Raman results. However, due to the different length scales analysed by the two techniques, the “moganite content” in microcrystalline SiO2 samples measured by Raman spectroscopy (short-range order) was found to be considerably higher than the “moganite content” measured by X-ray diffractometry (long-range order). The difference is explained by the presence of moganite nanocrystals, nano-range moganite lamellae, and single Brazil-law twin-planes that are detected by vibrational spectroscopy but that are not large enough (in the sense of coherently scattering lattice domains) to be detected by X-ray diffractometry. High resolution Raman analysis provides a measure of the moganite content and its spatial variation in microcrystalline silica samples with a lateral resolution in the μm-range. Variations in the moganite-to-quartz ratio are revealed by varying intensity ratios of the main symmetric stretching-bending vibrations (A1 modes) of α-quartz (465 cm−1) and moganite (502 cm−1), respectively. Traces of Raman microprobe analyses perpendicular to the rhythmic zoning of agates revealed that the moganite-to-quartz ratio is often not uniform but shows a cyclic pattern that correlates with the observed cathodoluminescence pattern (colour and intensity). Data obtained from an agate sample from a fluorite deposit near Okorusu, Namibia and from a volcanic agate from Los Indios, Cuba were selected for detailed presentation. Variations of cathodoluminescence and Raman data between single bands in agates suggest alternating formation of fine-grained, highly defective chalcedony intergrown with moganite, and coarse-grained low-defect quartz. Multiple zones indicate dynamic internal growth during a self-organizational crystallization process from silica-rich fluids.

Identification of pigments in a fourteenth-century miniature by combined micro-Raman and PIXE spectroscopic techniques

The pigments of a fourteenth-century miniature were analyzed through the combined efforts of two powerful spectroscopic techniques, particle-induced X-ray emission (PIXE) and micro-Raman. The use of these two complementary, non-destructive techniques provided more information than either method alone, permitting unambiguous identification of many of the pigments used in the creation of the miniature. The artist used a limited range of pigments, apparently preferring to use mixtures of materials rather than introduce additional pigments. A restoration to one area of the miniature used identical pigments to the original.