CL Microscopy Research Articles

Zebra dolomites of the Spessart, Germany: implications for hydrothermal systems of the European Zechstein Basin

Zebra dolomites have a distinctive texture and are a peculiar structural variety of dolostones often encountered in the vicinity of base metal deposits commonly in the Mississippi Valley-Type (MVT). We investigate origin and evolution of the zebra dolomites found in the region of the Spessart, northwestern Bavaria, Germany, through diagenetic and petrogenetic analysis using SEM, CL microscopy, O–C isotopes, and fluid inclusion micro-thermometry. Here, we aim to shed light on the nature of the fluids that altered the zebra dolomite of the Zechstein formation. We distinguish the geochemical signatures of two different fluid flow regimes post-dating texture formation, each characterized by specific homogenization temperatures and oxygen–carbon isotope ratios (Event 1: Th = 120 °C; δ18Ofluids = [0 to 2‰]; Event 2; Th = 300 °C; δ18Ofluids = 18‰). Comparison of these fluids and the associated mineralization with published regional fluid flow data support that the zebra dolomites in the Spessart most likely coincided with the Permian large-scale fluid flow event that occurred throughout the European Zechstein Basin.Graphical

Phase composition and genesis of pyroxenic jadeite from Guatemala: insights from cathodoluminescence.

Guatemalan jadeite has a long history, and much Guatemalan jadeite can be found on the market today with a variety of colors and species diversity. Seven varieties of green pyroxenic jadeite from Guatemala with greyish green, yellow green, brilliant green, blue green, dark green, black green and mottled green colors were investigated by combining the methods of XRD, Raman spectroscopy, cathodoluminescence, EPMA and μ-XRF mapping. The results showed that according to the composition, Guatemalan pyroxenic jadeite can be divided into three categories: jadeite jade, omphacite jade, and jadeite–omphacite jade. According to the characteristics of cathodoluminescence, it can be speculated that the formation of jadeite undergoes three stages, and the formation of jadeite jade is mainly due to the crystallization (Jad I) of the early jadeite fluid, along with the second-stage fluid metasomatism/crystallization (Jad II). In the later stage, the fluid that is rich in Ca–Mg–Fe components can replace early Jad I/Jad II, or it can coexist with Jad II, and metamorphism occurs to produce omphacite jade. The jadeite–omphacite jade can be formed when the omphacite fluid with incomplete metasomatism, with uneven texture and reduced transparency.

A study of secondary pyrite deformation and calcite veins in SAFOD damage zone with implications for aseismic creep deformation mechanism at depths >3 km

Previous studies of the San Andreas Fault damage-zone samples from the San Andreas Fault Observatory at Depth (SAFOD) have identified a variety of tectonic microstructures including pressure solution cleavage, calcite-sealed fractures vein fabric, and pyrite and anhydrite hydrothermal fracture sealing. Understanding the deformation provenance of the damage zone rocks and operative deformation mechanism(s) based on preserved microstructures provide insight into overall deformation behavior of the entire seismogenic zone in the creeping section of this transform fault. We analysed the deformation of hydrothermal secondary pyrite in connection with network of calcite veins in a sample of foliated ultracataclasites bordering the actively creeping Southwestern Deforming Zone (SDZ), using SEM, EBSD and CL microscopy. The results show that calcite veins associated with the pressure solution cleavage are crosscut by the secondary pyrite deformed under a range of P-T conditions. Relatively undeformed secondary pyrite is found sealing implosion microbreccia. Our review of previously available data indicates that the damage zone rocks may represent a collage of structural and compositional domains from both locked and creeping sections of the SAF. This interpretation together with results of this study suggest that weak-clay frictional deformation mechanism(s) is likely to be the predominant aseismic creep mechanism at depths below the SAFOD.

Cathodoluminescence of high‐pressure feldspar minerals as a shock barometer

AbstractCathodoluminescence (CL) analyses were carried out on maskelynite and lingunite in L6 chondrites of Tenham and Yamato‐790729. Under CL microscopy, bright blue emission was observed in Na‐lingunite in the shock veins. Dull blue‐emitting maskelynite is adjacent to the shock veins, and aqua blue luminescent plagioclase lies farther away. CL spectroscopy of the Na‐lingunite showed emission bands centered at ~330, 360–380, and ~590 nm. CL spectra of maskelynite consisted of emission bands at ~330 and ~380 nm. Only an emission band at 420 nm was recognized in crystalline plagioclase. Deconvolution of CL spectra from maskelynite successfully separated the UV–blue emission bands into Gaussian components at 3.88, 3.26, and 2.95 eV. For comparison, we prepared K‐lingunite and experimentally shock‐recovered feldspars at the known shock pressures of 11.1–41.2 GPa to measure CL spectra. Synthetic K‐lingunite has similar UV–blue and characteristic yellow bands at ~550, ~660, ~720, ~750, and ~770 nm. The UV–blue emissions of shock‐recovered feldspars and the diaplectic feldspar glasses show a good correlation between intensity and shock pressure after deconvolution. They may be assigned to pressure‐induced defects in Si and Al octahedra and tetrahedra. The components at 3.88 and 3.26 eV were detectable in the lingunite, both of which may be caused by the defects in Si and Al octahedra, the same as maskelynite. CL of maskelynite and lingunite may be applicable to estimate shock pressure for feldspar‐bearing meteorites, impactites, and samples returned by spacecraft mission, although we need to develop more as a reliable shock barometer.

High-resolution Campanian–Maastrichtian carbon and oxygen stable isotopes of bulk-rock and skeletal components: palaeoceanographic and palaeoenvironmental implications for the Boreal shelf sea

AbstractA high-resolution latest Early Campanian to Early Maastrichtian carbon and oxygen stable isotope record from the northern German Boreal shelf sea based on 537 analyses of co-occurring belemnites, brachiopods, inoceramids, oysters, and bulk rock samples is presented. All samples are precisely related to their stratigraphic, systematic and facies backgrounds and form an integrated, nearly 10-myr-long dataset with considerable palaeoenvironmental and palaeoceanographical implications. Petrographic studies indicate that low-magnesium calcitic coccoliths and calcispheres (i.e., planktic carbonate) predominate the bulk-rock data (marl-limestone rhythmites and chalks), thus representing a sea-surface water signal, and that only minor diagenetic alteration of the carbonate muds took place. Based on TL and CL microscopy, the investigated belemnites are extraordinarily well preserved, which may in part be explained by their early diagenetic surficial silicification (container effect), while the other macroinvertebrate groups are all less well preserved. The (plankton-dominated) δ13C values of the marl-limestone rhythmites and chalks (+1.1 to +2.5 ‰), recording a surface water signal, compare well with the δ18C data of inoceramids while δ13Cbrach. values (+1.5 to +3.0 ‰) are heavier than the bulk rock data. The large variation in the δ13Cbel. (-0.1 to +3.6 ‰) is attributed to isotopic disequilibrium of the biogenic carbonate formed by the belemnite animal. The bulk rock δ18O values show a remarkable low scatter, supporting petrographic observation of only minor diagenetic stabilisation/cementation, and can be approximated with northern German shelf sea-surface temperatures of ca. 20°C for the Late Campanian (ca. -2 ‰ δ18O), being slightly cooler during the Early Maastrichtian. The δ18O values of the belemnite rostra are even less variable and quite rich in heavier18O (-0.7 to +0.6 with a mean of -0.1 ‰ δ18Obel.) in comparison to bulk rock and other skeletal components. Based on their excellent microstructural preservation and non-luminescence, we conclude that the belemnite rostra are diagenetically unaltered and have preserved the primary δ18O signal of ambient seawater (12 ± 2°C). In the absence of any indication for migration from cooler water masses and evidence for authochtonous populations we assume that the belemnites of the genera Belemnitella and Belemnella lived as nektobenthos near the sea-floor and thus record the temperature of the bottom mixed layer of the seasonally weakly stratified north German shelf sea at water depths of 100 to 150 m; the temperature gradient was thus 12.5-18.75 m/1°C. A conspicuous latest Campanian cooling event is evident in both sea-surface and bottom-water temperatures. The δ18O values of nearly all investigated benthic fossils lie between the isotope values of pristine belemnites and bulk rock, and, therefore, should be used for palaeotemperature reconstructions only with great care.

Correlative near-infrared light and cathodoluminescence microscopy using Y2O3:Ln, Yb (Ln = Tm, Er) nanophosphors for multiscale, multicolour bioimaging.

This paper presents a new correlative bioimaging technique using Y2O3:Tm, Yb and Y2O3:Er, Yb nanophosphors (NPs) as imaging probes that emit luminescence excited by both near-infrared (NIR) light and an electron beam. Under 980 nm NIR light irradiation, the Y2O3:Tm, Yb and Y2O3:Er, Yb NPs emitted NIR luminescence (NIRL) around 810 nm and 1530 nm, respectively, and cathodoluminescence at 455 nm and 660 nm under excitation of accelerated electrons, respectively. Multimodalities of the NPs were confirmed in correlative NIRL/CL imaging and their locations were visualized at the same observation area in both NIRL and CL images. Using CL microscopy, the NPs were visualized at the single-particle level and with multicolour. Multiscale NIRL/CL bioimaging was demonstrated through in vivo and in vitro NIRL deep-tissue observations, cellular NIRL imaging, and high-spatial resolution CL imaging of the NPs inside cells. The location of a cell sheet transplanted onto the back muscle fascia of a hairy rat was visualized through NIRL imaging of the Y2O3:Er, Yb NPs. Accurate positions of cells through the thickness (1.5 mm) of a tissue phantom were detected by NIRL from the Y2O3:Tm, Yb NPs. Further, locations of the two types of NPs inside cells were observed using CL microscopy.

Bright luminance from silicon dioxide film with carbon nanotube electron beam exposure

We observed the bright bluish-white luminescence with naked eye from carbon nanotube electron beam exposed silicon dioxide (SiO2) thin film on Si substrate. The luminescence shows a peak intensity at 2.7eV (460nm) with wide spread up to 600nm after the C-beam exposed on SiO2 thin film. The C-beam exposure system is composed of carbon nanotube emitters as electron beam source. The brightness strongly depend on the exposure condition. Luminescence characteristic was optimized by C-beam adjustment to observe with the naked eye. The cause of luminescence in the C-beam exposed SiO2 thin film is analyzed by CL microscopy, FT-IR, AFM and ellipsometer. Decrease of Si–O bonding was observed after C-beam exposure, and this reveals that oxygen deficient defects which are irradiation-sensitive cause 2.7eV peak of luminescence.

Diagenetic history of lower Pliocene rhodoliths of the Azores Archipelago (NE Atlantic): Application of cathodoluminescence techniques

The diagenetic history of calcareous fossils is required for their application as palaeoenvironmental indicators. In this study, cathodoluminescence-microscopy (CL microscopy) and back scatter electron image–energy dispersive X-ray spectroscopy (BSE–EDS microscopy) were applied to Pliocene rhodoliths from the Azores Archipelago (NE Atlantic) in order to gain additional insight regarding the trace element content distribution throughout the algae thalli, and to ascertain palaeoenvironmental interpretations.Two types of luminescence were obtained: (1) high and (2) low luminescence. Rhodoliths with high luminescence are related with high concentrations of Mn2+ in seawater and low luminescence rhodoliths are related with low concentrations of Mn2+ in seawater. When the rhodoliths were deposited at about 4.0–4.5Ma, the shoreline configuration of Santa Maria Island was much different than today. The influence of volcanic activity due to the extrusion of lavas and associated products and/or the presence of active shallow-water hydrothermal vents, was reflected in the sea water chemistry, with penecontemporaneous palaeoshores of the island featuring a high sea water concentration of Mn2+, which mirrored on the rhodolith Mn2+ high concentration. By contrast, rhodoliths located about 2.8 and 2.9km from the shore, in areas with low seawater Mn2+ concentration, had low luminescence, reflecting the low Mn2+ concentration in seawater. Rhodoliths chemical data and the geological history of the island proved to be congruent with the palaeogeographical reconstruction of Santa Maria Island at the time of the formation of the rhodoliths.

Cathodoluminescence (CL) and electron paramagnetic resonance (EPR) studies of clay minerals

¶Sheet silicates of the serpentine–kaolin-group (serpentine, kaolinite, dickite, nacrite, halloysite), the talc–pyrophyllite-group (talc, pyrophyllite), the smectite-group (montmorillonite), and illite (as a mineral of the mica-group) were investigated to obtain information concerning their cathodoluminescence behaviour. The study included analyses by cathodoluminescence (CL microscopy and spectroscopy), electron paramagnetic resonance (EPR), X-Ray diffraction (XRD), scanning electron microscopy (SEM) and trace element analysis.

Upper Triassic reef facies in the Asher-Atlit-1 borehole, Northern Israel: Microfacies, cement stratigraphy and paleogeographic implications

The late Triassic succession of the Asher-Atlit 1 borehole is over 1000 m thick, and is composed of reefal and associated facies interbedded with volcanics of Norian age. Only borehole cuttings are available. Microfacies classification and cement stratigraphy determined by optical and CL microscopy, allowed discrimination of six episodes of reef establishment, progradation, shallowing, and termination. Organic buildups are constructed of reef-building biota (sponges, possible corals, encrusting organisms) typical for the late Triassic of the Tethys. Reef-associated facies include fore-slope, central reef, ooid shoal, lagoonal, and supratidal environments. Cement zoning patterns trace diagenetic signatures which range from early neomorphic skeletal replacements and original marine cements, via characteristic burial sequences; depositional and diagenetic sequences are terminated by marginal marine intra- or supratidal conditions, and subaerial exposure with pedogenic overprints. Volcanic episodes tend to be associated with termination of carbonate sedimentation episodes, while volcanic quiescence and subsidence permit vertical progradation of reefal and associated facies. The depositional and progradational environment, rapid rate of sedimentation, periodicity, association with volcanics, and regional considerations, suggest a depositional setting on the rifted shelf-margin of the nascent Neo-Tethys, with a possible eustatic overprint.

Optical and structural characterization of a self-aligned single electron transitor structure by cathodoluminescence microscopy

We report about optical and structural investigations of a self-aligned single electron transistor (SET) structure using cathodoluminescence-(CL) and transmission electron microscopy (TEM). The SET structures were fabricated by MBE growth of GaAs/AlAs on different prepatterned GaAs (100) substrates. This technique for the in situ formation of nanoscopic semiconductor heterostructures is presently a widely used and promising approach for the fabrication of low-dimensional systems like quantum wires and quantum dots (QD). The active region of the SET structure consists of a GaAs/AlGaAs-QD formed by thickness modulation of a single quantum well (SQW) during the MBE growth. The position and the size of the QD is defined by the design of the substrate pattern. The thickness modulation of the GaAs-SQW is evidenced by TEM investigations. The lateral confinement potential given by the thickness modulation of GaAs-SQW is directly imaged by CL microscopy.

Epitaxial lateral overgrowth of GaN structures: spatially resolved characterization by cathodoluminescence microscopy and micro-Raman spectroscopy

The epitaxial lateral overgrowth of GaN structures is comprehensively characterized by scanning cathodoluminescence microscopy and micro-Raman spectroscopy. The samples under study consist of a 3-μm thick GaN buffer layer grown by MOVPE on (0001) sapphire and subsequently structured using a SiO 2 mask. The resulting stripe pattern is overgrown with HVPE GaN. Mask orientations along 〈 1 100 〉 and 〈 11 20 〉 are compared. CL microscopy directly visualizes the significant differences between the overgrown areas on top of the SiO 2-mask and the coherently grown regions between the SiO 2-stripes. The overgrown GaN shows a blue shift and a strong broadening of the luminescence. In contrast, the local luminescence from the areas of coherent (0001)-growth is dominated by narrow excitonic emission. The CL results are correlated with micro-Raman spectroscopy yielding information on the local strain and free carrier concentration.

High-resolution cathodoluminescence combined with SHRIMP ion probe measurements of detrital zircons

AbstractCathodoluminescence (CL) microscopy and spectroscopy combined with SHRIMP ion probe measurements were carried out on detrital zircons from the Cretaceous Weferlingen quartz sand (Germany) to distinguish and characterize different zircon populations.Investigations by CL microscopy, SEM-CL and BSE imaging show that there are three main types of zircons (general grain sizes of 100–200 µm): (1) apparently weakly zoned, rounded grains with relict cores, (2) well rounded fragments of optically more or less homogeneous zircon grains showing CL zoning predominantly parallel to the z-axis, and (3) idiomorphic to slightly rounded zircon grains typically showing oscillatory euhedral CL zoning. A fourth type of low abundance is characterized by well-rounded grain fragments with an irregular internal structure showing bright yellow CL.High-resolution CL spectroscopic analyses reveal that blue CL is mainly caused by an intrinsic emission band centered near 430 nm. Dy3+ is the dominant activator element in all zircons, whereas Sm3+, Tb3+, Nd3+ have minor importance. Yellow CL (emission band between 500 and 700 nm) is probably caused by electron defects localized on the [SiO4] groups (e.g. related to oxygen vacancies) or activation by Yb2+ generated by radiation. Variations of the integral SEM-CL intensity are mainly controlled by the intensity of the broad bands and the Dy3+ peaks.SHRIMP analysis provides in situ high-resolution U-Pb dating of single zircon grains and confirms different ages for the evaluated different zircon types. The measurements show that the U-Pb ages of the zircons from Weferlingen scatter over a wide range (340 to 1750 Ma), backing up earlier conclusions that the quartz sand from Weferlingen is quite heterogeneous in terms of provenance.

Recognition and Distribution of A(g) and B(g) Dislocations in Indentation Deformation Zones on {111} and {110} Surfaces of CdTe

The distributions of polar dislocations appearing in surface and volume deformation zones of indentations on 111†Cd, 1 1 1†Te and 110† surfaces of CdTe bulk crystals are studied. Distinct CL contrast properties proved in CdTe for A(g)and B(g)-type dislocations are utilised to recognise Cd(g) and Te(g) dislocation segments in the deformation-induced defect configurations. The microscopic spatial glide geometries as caused by indenting the low-indexed surfaces are theoretically developed within the framework of an advanced h110i glide prism model. Comprehensive results gained by means of depth-resolved CL microscopy fully confirm the concept of 3D glide prism formation. The experimental findings give evidence for a coexistence of Cd(g) and Te(g) dislocations in tangential as well as tetrahedral deformation zones. From that, correlated propagation of polar dislocation segments during plastic flow has to be concluded.

Characterization of GaN Films on Sapphire by Cathodoluminescence

ABSTRACTCathodoluminescence (CL) spectroscopy and microscopy were used to study the luminescent properties of a variety of GaN films, both Si-doped and unintentionally-doped, grown on sapphire substrates. A narrow and intense near band-edge emission was found in the CL spectrum of each film examined, and deep-level emission was also observed for some of the films. The luminescence efficiency of near band-edge emission increased with a faster rate than that of deep-level emission when the pumping current was increased. Spatial nonuniformities of luminescence were observed in monochromatic CL microscopy, and microstructures were observed in scanning electron microscopy. No correlations between luminescence features and microstructural features were seen. Degradation of near band-edge luminescence was observed, accompanied by growth of deep-level emission.

Constraining Authigenic Quartz Precipitation from CL Microscopy and Trace Element Geochemistry: ABSTRACT

Constraining Authigenic Quartz Precipitation from CL Microscopy and Trace Element Geochemistry: ABSTRACT

Defect Analysis In Substrate Materials for High Tc Superconducting Thin Films

AbstractMany defects in high Tc superconducting films propagate from the substrate through to the film surface, disturbing the epitaxy at the interface and adversely affecting the physical properties of the film, particularly Jc. In this study the surface of Magnesium Oxide (100) single crystal substrates with different preparative treatments have been investigated using optical cathodoluminescence microscopy (CL), with a view to establishing its effect on the deposition of thin films of YBa2Cu3O7-δ superconductors.CL excitations due to mechanically and chemically induced defects in the MgO substrate crystals are observed by optical CL microscopy. Several pre-deposition treatments have been compared in this way to determine the best preparation route for the substrates. Jc measurements indicate that the substrate surface quality is an important parameter in the production of high quality thin films especially for the fabrication of devices.It is concluded that CL provides a powerful and rapid tool for MgO quality assessment before thin film deposition.

A modification for improved electron gun current control in cold cathode Cl microscopy

A modification for improved electron gun current control in cold cathode Cl microscopy