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At least 271 records · Page 15

Using Xe Plasma FIB for High-Quality TEM Sample Preparation

Here, a direct comparison between electron transparent transmission electron microscope (TEM) samples prepared with gallium (Ga) and xenon (Xe) focused ion beams (FIBs) is performed to determine if equivalent quality samples can be prepared with both ion species. We prepared samples using Ga FIB and Xe plasma focused ion beam (PFIB) while altering a variety of different deposition and milling parameters. The samples’ final thicknesses were evaluated using STEM-EELS $\textit{t/λ}$ data. Using the Ga FIB sample as a standard, we compared the Xe PFIB samples to the standard and to each other. We show that although the Xe PFIB sample preparation technique is quite different from the Ga FIB technique, it is possible to produce high-quality, large area TEM samples with Xe PFIB. We also describe best practices for a Xe PFIB TEM sample preparation workflow to enable consistent success for any thoughtful FIB operator. For Xe PFIB, we show that a decision must be made between the ultimate sample thickness and the size of the electron transparent region.

47 OTHER INSTRUMENTATION↗

Real-time tracking of structural evolution in 2D MXenes using theory-enhanced machine learning

In situ Electron Energy Loss Spectroscopy (EELS) combined with Transmission Electron Microscopy (TEM) has traditionally been pivotal for understanding how material processing choices affect local structure and composition. However, the ability to monitor and respond to ultrafast transient changes, now achievable with EELS and TEM, necessitates innovative analytical frameworks. Here, we introduce a machine learning (ML) framework tailored for the real-time assessment and characterization of in operando EELS Spectrum Images (EELS-SI). We focus on 2D MXenes as the sample material system, specifically targeting the understanding and control of their atomic-scale structural transformations that critically influence their electronic and optical properties. This approach requires fewer labeled training data points than typical deep learning classification methods. By integrating computationally generated structures of MXenes and experimental datasets into a unified latent space using Variational Autoencoders (VAE) in a unique training method, our framework accurately predicts structural evolutions at latencies pertinent to closed-loop processing within the TEM. This study presents a critical advancement in enabling automated, on-the-fly synthesis and characterization, significantly enhancing capabilities for materials discovery and the precision engineering of functional materials at the atomic scale.

47 OTHER INSTRUMENTATION↗

Inter-species interconnections in acid mine drainage microbial communities

Metagenomic studies are revolutionizing our understanding of microbes in the biosphere. They have uncovered numerous proteins of unknown function in tens of essentially unstudied lineages that lack cultivated representatives. Notably, few of these microorganisms have been visualized, and even fewer have been described ultra-structurally in their essentially intact, physiologically relevant states. Here, we present cryogenic transmission electron microscope (cryo-TEM) 2D images and 3D tomographic datasets for archaeal species from natural acid mine drainage (AMD) microbial communities. Ultrastructural findings indicate the importance of microbial interconnectedness via a range of mechanisms, including direct cytoplasmic bridges and pervasive pili. The data also suggest a variety of biological structures associated with cell-cell interfaces that lack explanation. Some may play roles in inter-species interactions. Interdependences amongst the archaea may have confounded prior isolation efforts. Overall, the findings underline knowledge gaps related to archaeal cell components and highlight the likely importance of co-evolution in shaping microbial lineages.

Thermoplasmatales↗

Bulk Current Injection Testing of Cable Noise Reduction Techniques, 50 kHz to 400 MHz

This paper presents empirical results of cable noise reduction techniques as demonstrated using bulk current injection (BCI) techniques with radiated fields from 50 kHz - 400 MHz. It is a follow up to the two-part paper series presented at the Asia Pacific EMC Conference that focused on TEM cell signal injection. This paper discusses the effects of cable types, shield connections, and chassis connections on cable noise. For each topic, well established theories are compared with data from a real-world physical system.

Bradley, Arthur T.↗

In-situ TEM investigation of void swelling in nickel under irradiation with analysis aided by computer vision

Understanding the stability of irradiation-induced voids in materials is important for engineering material's swelling behavior under irradiation. In-situ TEM offers a spatial and temporal resolution that is suitable for investigating the evolution of voids under irradiation. However, the in-situ videos have often been too large to be analyzed manually, leaving the valuable data underutilized. For this work, we developed a deep learning-based semantic segmentation model to consistently study the growth and shrinkage of voids in nickel under 1 MeV krypton ion irradiation at various temperatures from 525 °C to 650 °C. With a foil thickness near 100 nm and ion flux of 6.3 × 10 11 ions∙ cm –2 ∙s –1 , the pre-existing voids, which were created beforehand by irradiation at 600 °C to 0.5 dpa, shrank at low temperatures and grew at high temperatures under irradiation, where the transition occurred at 575 °C (~0.5 T M ). The observed stability transition provided new insight for the shrinkage mechanism of voids under irradiation. In addition, an annealing experiment on nickel, previously irradiated at 600 °C to 3 dpa, was performed sequentially at 650 °C to 720 °C to reveal the shrinkage rate of void as a function of temperature and void size. The advantage of combining computer vision and in-situ TEM to obtain comprehensive void evolution was demonstrated.

36 MATERIALS SCIENCE↗

Structural and transport properties of NdCrO{sub 3} nanoceramics

Reitveld refinement of the room temperature powder X-ray diffraction profile of NdCrO{sub 3} (NCO) nanoceramics synthesized by sol-gel processing shows orthorhombic Pnma (D{sub 2h}{sup 16}) space group symmetry. The refined lattice parameters are a = 5.482(3) A, b = 7.689(4) A and c = 5.416(3) A. Transmission electron microscopy (TEM) of NCO shows that the average particle size is around 70 nm. The electrical transport property of NCO is investigated by both conductivity and electric modulus formalism. The electrical data is taken by a LCR meter in a temperature range from 303 K to 573 K and in a frequency range from 42 Hz to 1.1 MHz. The ac conductivity follows a power law. The Cole-Cole plot of impedance at 303 K shows grain effect.

36 MATERIALS SCIENCE↗

Matrix and fine-grained rims in the unequilibrated CO3 chondrite, ALHA77307 - Origins and evidence for diverse, primitive nebular dust components

SEM, TEM, and electron microprobe analysis were used to investigate in detail the mineralogical and chemical characteristics of dark matrix and fine-grained rims in the unequilibrated CO3 chondrite ALHA77307. Data obtained revealed that there was a remarkable diversity of distinct mineralogical components, which can be identified using their chemical and textural characteristics. The matrix and rim components in ALHA77307 formed by disequilibrium condensation process as fine-grained amorphous dust that is represented by the abundant amorphous component in the matrix. Subsequent thermal processing of this condensate material, in a variety of environments in the nebula, caused partial or complete recrystallization of the fine-grained dust.

Brearley, Adrian J.↗

Microstructural Characterization of Irradiated U{sub 0.17}ZrH{sub 1.6} Using Ultrasonic Techniques

In recent years, there has been an increased level of effort to understand the changes in microstructure that occur due to irradiation of nuclear fuel. The primary driver for this increased effort is the potential for designing new fuels that are safer and more reliable, in turn enabling new and improved reactor technologies. Much of the data on microstructural change in irradiated fuels is generated through a host of post irradiation examination techniques such as optical microscopy (OM), scanning electron microscopy (SEM), and transmission electron microscopy (TEM) to determine grain structure, porosity, crack geometry, etc. in irradiated fuels. Such 'traditional' examination techniques were recently used to characterize a novel new fuel consisting of U{sub 0.17}ZrH{sub 1.6} pellets bonded to zircaloy-2 cladded with lead-bismuth eutectic before and after irradiation. In addition to the conventional suite of post-irradiation examination tools, several nondestructive interrogation techniques exist which bring the potential for in-situ assessment of microstructural changes. One such method, ultrasonic examination, was tested on each of the samples. This paper describes the results of this examination. Ultrasonic measurements have a long and successful history of use for nondestructive materials characterization, including nondestructive evaluation (NDE) of degradation and damage, microstructure characterization, and measurement of physical parameters for process control. Ultrasonic NDE is critical to the nuclear power industry's in-service inspection program for maintaining pressure boundary integrity, and is being actively investigated for PIE of fuels. Ultrasonic measurements, typically performed at 10 MHz or higher, performed post irradiation show that fuel microstructural parameters, such as porosity and grain size, can be correlated to ultrasonic velocity. The objective of this examination was to assess the feasibility of using ultrasonic measurements on irradiated fuel to determine sensitivity to microstructural changes.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Martian B Storm Genesis and Evolution: Initial Analysis of Thermal Datasets.

Introduction: Dust lifting on Mars likely occurs primarily as a result of the exchange of momentum between the atmosphere and the surface via saltation. During saltation, sand-sized particles are mobilized but do not enter into suspension. When these larger particles fall back to the surface, kinetic energy is transferred to smaller dust particles which are then lofted into suspension in the atmosphere. Depending on the altitude to which dust is lofted, it can have a significant effect on atmospheric temperatures. As a strong absorber and emitter in the infrared, dust can influence atmospheric heating and modify the global circulation and weather on Mars [1,2]. Although dust is present in Mars’ atmosphere throughout the year, the atmosphere is generally dustier during the second half of the year when Mars is near perihelion. Observations reveal that episodic global-scale dust storms and fairly regular regional-scale dust storms are superimposed on a well-defined and highly repeatable seasonal cycle of dust opacity and associated mid-level atmospheric temperature responses. Kass et al. (2016) used 50 Pa temperature observations from MRO/MCS to identify three highly repeatable time periods during which regional dust storms occur, and designated them the “A”, “B” and “C” storms. While “A” and “C” storms have been studied a fair amount to-date, “B” storms have not yet been investigated in detail. This study explores the generation and evolution of the annually recurring regional dust storm known as the “B” storm, which was identified and categorized by Kass et al. (2016) based on 25 km (50 Pa) temperature observations. The B storm is a southern-hemisphere (SH) phenomenon that originates at the cap edge just after perihelion and which reaches peak intensity during the SH summer solstice, Ls 270. It may originate from the cap edge storms that spawn near the edge of the seasonal CO2 cap during retreat, but the mechanisms for B storm genesis have yet to be determined definitively [1]. Methods: We will use observational data sets and a global climate model (GCM) to investigate “B” regional storms. The data analysis component will include the analysis of imagery from MGS/MOC and MRO/MARCI, and spectroscopic data sets of dust and temperatures from MGS/TES and MRO/MCS with the goal of fully characterizing the behavior of these storms. Both MGS and TES provide data well-suited for temperature analysis at 25 km. MCS measures atmospheric temperature, dust extinction, and water ice extinction at 5 km intervals from the surface to about 80 km. TES measured atmospheric temperatures, column dust and water ice opacities, and column water vapor abundances. Measurements made by TES extended from the surface to about 40 km [1]. At the 50 Pa (25 km) level, local dust events usually confined to shallower depths are effectively filtered out of the analysis leaving the regional dust events identifiable by their temperature signatures [1]. Our preliminary analysis makes use of the fact that the brightness temperature at 15 microns (T15 temperature) is a close approximation to observed temperature at 25 km. We first reproduce the zonal mean 50 Pa level temperature plots for MY 29-32 to establish a baseline for our procedures moving forward [1]. Expanding on Kass et al. (2016), we include recent MCS data from MY 33 and 34 as well. Preliminary Analysis: The daytime (3PM) T15 temperatures in Figure 1 indicate: in MY 29, a strong A storm at Ls 240, a B storm at high southern latitudes just after Ls 270, and a C storm at Ls 320; in MY 30, a B storm at Ls 270; in MY 31 & MY 32, a B storm just before Ls 270; in MY 33, a B storm at Ls 270; and in MY 34, a strong A storm in the northern hemisphere at Ls 210, and a B storm around Ls 270 although there is a data gap. For the B storms, each is indicative of lofted dust and resultant warming. The daytime temperature structure illustrates that the B storm occurs annually around Ls 270 and is confined to high southern latitudes. It reaches its peak intensity around SH summer solstice, Ls 270, consistently for all six MY assessed. Since direct solar heating is absent overnight, the nighttime T15 temperatures (Figure 2) are often useful for differentiating the heat signature of direct solar heating from the dynamical response to that heating. However, in the southern polar latitudes at perihelion the sun does not set and direct solar heating remains present throughout the night. Importantly for our study, dust lofted in the B storm experiences this direct heating day and night for the entirety of its lifetime. The B storm expands as far north as -60 latitude and decays in latitudinal extent more gradually than it grows. This feature is less obvious in the nighttime (3AM) T15 temperatures (Figure 2). The temperature signal is stronger at night for MY 30-33. The warm pool is larger in area relative to the background at night in these four cases. This more uniform warming masks the “tail” feature somewhat, such that it is barely noticeable during these years. Unfortunately, gaps in MCS data in MY 29 and 34 prevent confirmation of the tail feature during those years, however, the B storm temperature signature follows a very different pattern than that described for MY 30-33. MY 29 and 34 appear to show smaller centers of warming at night and larger centers of warming during the day. This is in opposition to that previously described for MY 30-33. Conclusions and Future Work: We will continue investigating the heat signatures of B storms by looking at the total column heating as recorded by TES. We will also look at lower altitudes for patterns that may describe the relationship between B storms and the cap edge storms that develop while the seasonal cap is retreating. In the future, we will use GCM simulations to determine the atmospheric and thermo-dynamic conditions associated with these storms.

Courtney Marylou Batterson↗

Characterizing the nano-structure and defect structure of nano-scaled non-ferrous structural alloys

The presence and interaction of nanotwins, geometrically necessary dislocations, and grain boundaries play a key role in the mechanical properties of nanostructured crystalline materials. Therefore, it is vital to determine the orientation, width and distance of nanotwins, the angle and axis of grain boundary misorientations as well as the type and the distributions of dislocations in an automatic and statistically meaningful fashion in a relatively large area. In this paper, such details are provided using a transmission electron microscope-based orientation microscopy technique called ASTAR™/precession electron diffraction. The remarkable spatial resolution of this technique (~ 2 nm) enables highly detailed characterization of nanotwins, grain boundaries and the configuration of dislocations. This orientation microscopy technique provides the raw data required for the determination of these parameters. The procedures to post-process the ASTAR™/PED datasets in order to obtain the important (and currently largely hidden) details of nanotwins as well as quantifications of dislocation density distributions are described in this study. - Highlights: • EBSD cannot characterize defects such as dislocations, grain boundaries and nanotwins in severely deformed metals. • TEM based orientation microscopy technique called ASTAR™/PED was used to resolve the problem. • Locations and orientations of nanotwins, dislocation density distribution and grain boundary characters can be resolved. • This work provides the bases for further studies on the interactions between dislocations, grain boundaries and nanotwins. • The computation part is explained sufficiently which helps the readers to post process their own data.

36 MATERIALS SCIENCE↗

Phase relations and structural features in the system Ni-Zn-B

Phase relations for the system Ni-Zn-B have been established in the isothermal section at 800 Degree-Sign C based on X-ray powder diffraction and electron microprobe analyses of about 60 samples, which have been prepared by hot pressing of pre-annealed powder compacts of arc-melted master alloys Ni{sub x}B{sub y} and Zn-filings. Six ternary compounds (labeled {tau}{sub 1} to {tau}{sub 6}) were found to exist, which in some cases exhibit considerable mutual solid solubilities mostly as an exchange of Ni-Zn at constant B-content, but in the case of the so-called {tau}-phase {tau}{sub 1}-(Ni{sub 1-x}Zn{sub x}){sub 21}[Zn{sub 1-y-z}{open_square}{sub y}(B{sub 4}){sub z}]{sub 2}B{sub 6} (0.07{<=}x{<=}0.11, 0.07{<=}y{<=}0.53, 0{<=}z{<=}0.3) also with Zn/B substitution. Single crystal X-ray data analysis for the composition x=0.07, y=0.125, z=0.30, and a=1.05800(3) nm confirmed the Cr{sub 23}C{sub 6} type with space group Fm3{sup Macron }m, but revealed partial replacement of Zn-atoms by B{sub 4}-tetrahedra (R{sub F}=0.014). Whereas Ni/Zn exchange (at constant B-content) ranges at about 4-5 at% for {tau}{sub 4}-Ni{sub 3}ZnB{sub 2} and {tau}{sub 5}-Ni{sub 48}Zn{sub 32}B{sub 20}, it is below 3 at% for {tau}{sub 2}-Ni{sub 12}ZnB{sub 8-x} (x=0.43), {tau}{sub 3}-Ni{sub 21}Zn{sub 2}B{sub 20} and {tau}{sub 6}-Ni{sub 47}Zn{sub 23}B{sub 30}. The crystal structures of {tau}{sub 2}-Ni{sub 12}ZnB{sub 8-x} (x=0.43; Ni{sub 12}AlB{sub 8} type), {tau}{sub 3}-Ni{sub 21}Zn{sub 2}B{sub 20} (own type) and {tau}{sub 4}-Ni{sub 3}ZnB{sub 2} (own type) have been determined in our foregoing paper [8]. Due to the non-availability of suitable single crystals, the crystal structures of {tau}{sub 5}-Ni{sub 48}Zn{sub 32}B{sub 20} (body-centered orthorhombic; a=1.6(2) nm, b=0.63(7) nm, and c=0.27(0) nm, determined from TEM) and of {tau}{sub 6}-Ni{sub 47}Zn{sub 23}B{sub 30} have not been elucidated yet. Phase equilibria at 800 Degree-Sign C are dominated by a large three-phase field ({beta}B)+Ni{sub 2}Zn{sub 11}+{tau}{sub 3}, as practically all ternary compounds form at compositions with less than about 50 at% Ni. Furthermore, precise data on atom site distribution and positional parameters have been provided from X-ray single crystal refinements for Ni-borides, for which crystal structures hitherto have only been derived from X-ray diffraction photographs: o-Ni{sub 4}B{sub 3-x} (x=0.19; Pnma, a=1.9665(4) nm, b=0.29852(1) nm, c=0.65750(2) nm; R{sub F}=0.015) and m-Ni{sub 4}B{sub 3} (C2/c, a=0.64356(3) nm, b=0.48867(3) nm, c=0.78267(3) nm, {beta}=103.288(3) Degree-Sign , R{sub F}=0.021). - Graphical abstract: Ni-Zn-B isothermal section at 800 Degree-Sign C. Highlights: Black-Right-Pointing-Pointer Phase relations were determined for the system Ni-Zn-B at 800 Degree-Sign C. Black-Right-Pointing-Pointer Existence of six ternary compounds ({tau}{sub 1}-{tau}{sub 6}) has been confirmed at 800 Degree-Sign C. Black-Right-Pointing-Pointer Homogeneity range for {tau}{sub 1} with respect to Ni/Zn and Zn/B at 800 Degree-Sign C has been determined. Black-Right-Pointing-Pointer The crystal structures of {tau}{sub 5}-Ni{sub 48}Zn{sub 32}B{sub 20} from TEM (oI, a=1.6(2) nm, b=0.63(7) nm, and c=0.27(0) nm). Black-Right-Pointing-Pointer Precise data on {tau}{sub 1}-(Ni{sub 1-x}Zn{sub x}){sub 21}[Zn{sub 1-y-z{open_square}y}(B{sub 4}){sub z}]{sub 2}B{sub 6} (0.07{<=}x{<=}0.11, 0.07{<=}y{<=}0.53, 0{<=}z{<=}0.3), o-Ni{sub 4}B{sub 3-x} and m-Ni{sub 4}B{sub 3} have been presented.

36 MATERIALS SCIENCE↗

Laboratory Studies of Solid Carbon Dioxide in Planetary and Interstellar Ices

Laboratory spectra have shown that CO2. is a powerful diagnostic tool for analyzing infrared data from remote observations, as it has been detected on icy moons in the outer solar system as well as dust grain surfaces in the interstellar medium. IR absorption profiles of CO2 wi thin ice mixtures containing H2O and CH30H change with respect to tem perature and mixture ratios. In this particular study, the CO2 stretch mode around 235O cm (exp -1) (4.3 rricrons) is systematically observ ed in different mixtures with H2O and CH30H in temperature ranges from 15K to 150 K, as well as vibrational modes in the near-IR such as th e combination bands near 3700 cm (exp -1) (2.7 microns) and 5080 (exp -1) (2.0 microns). Additionally, some high?temperature deposits (T > 50 K) of H2O, CH30H, and CO2 ice mixtures were performed to determine the maximum temperatures at which CO2 will deposit on the sample win dow. These data may then be used to interpret spectra obtained from remote IR observations. This research was sponsored by Oak Ridge Associ ated Universities (ORAU) through the NASA Postdoctoral Program (NPP) as well as Ames Research Center and the SETI institute who provided fa cilities and equipment.

White, Douglas↗

Growth of faceted SiC nanostructures using vapor phase condensation: Microstructural analysis

Highlights: • Synthesis of nanocrystalline SiC using thermal plasma route. • XRD data indicates presence of both α- and β-SiC polytypes with β-SiC as the major content. • HRTEM and SAED analysis reveals polytypic arrangement with stacking faults SiC nanoparticles. • TEM micrograph reveals presence of faceted structures such as hexagonal, triangular, triangular pyramidal structure. - Abstract: The paper emphasizes the morphological and microstructural analysis of SiC nanostructures grown by thermal plasma assisted gas phase condensation process. High Resolution Transmission Electron Microscopic and Selected Area Electron Diffraction studies are used to analyze the growth directions and the polytypic arrangement with stacking faults in the as synthesized SiC nanoparticles. The results help in understanding the hierarchical poly-types related to the observed geometries and showed the presence of both α- and β-SiC polytypes. The microstructural study is supported by X-Ray diffraction and UV–Visible absorption spectroscopic studies.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Information depth in backscattered electron microscopy of nanoparticles within a solid matrix

Highlights: • Backscattered electron microscopy was used for reliable determination of nanoparticle density and sizes within Al alloys • Backscattered electron information depth was determined as a function of nanoparticle size from Monte Carlo simulations • Unlike transmission electron microscopy, the method is non-destructive and allows analyzing large sample areas • Good agreement with transmission electron microscopy data shows that our method is suitable for nanocomposite materials - Abstract: Measuring the dimensions and number density of nanoparticles dispersed in a solid matrix is usually accomplished via transmission electron microscopy (TEM) which suffers from high cost, low throughput, and small analytical volume. In comparison, scanning backscattered electron microscopy is inexpensive, requires little sample preparation, and allows for the analysis of large sample areas. However, the information depth is usually not known precisely and depends on several factors such as the composition of the nanoparticles and the matrix as well as the size of the nanoparticles, hindering the reconstruction of the actual size distribution and three-dimensional number density. Here we present a method to estimate the information depth for spherical nanoparticles of different sizes in order to accurately determine size distribution and number density. The approach is based on Monte Carlo simulation of electron trajectories in the material and analysis of the obtained backscattered electron signal-to-noise-ratio. Our experimental results are compared to those obtained via TEM and good agreement is demonstrated; this shows that TEM can be replaced by scanning electron microscopy for studying nanocomposites in many cases.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Seasonal cycle of the residual mean meridional circulation in the stratosphere

The transformed Eurlerian-mean (TEM) residual circulation is used to study the zonally averaged transport of mass in the stratosphere. The residual circulation is estimated from heating rates computed with a radiative transfer model using data from the Upper Atmosphere Research Satellite (UARS) as inputs. An annual cycle exists in the resulting circulation in the lower stratosphere, with a larger net upward mass flux across a pressure surface in the tropics during northern hemisphere winter than during northern hemisphere summer. The annual cycle in upward tropical mass flux follows the annual cycle in downward mass flux across a pressure surface in the northern hemisphere extratropics. It is argued that the annual cycle in zonal momentum forcing in the northern hemisphere stratosphere is controlling mass flux across a pressure surface in the lower stratosphere both in the tropics and in the northern hemisphere extratropics.

Rosenlof, Karen H.↗

Exploring dynamic surface processes during silicate mineral (wollastonite) dissolution with liquid cell

Most liquid cell transmission electron microscopy (LC TEM) studies focus on nanoparticles or nanowires, in large part because the preparation and study of materials in this size range is straightforward. By contrast, this is not true for samples in the micrometre size range, in large part because of the difficulties associated with sample preparation starting from a ‘bulk’ material. There are also many advantages inherent to the study of micrometre-sized samples compared to their nanometre-sized counterparts. Here, we present a liquid cell transmission electron study that employed an innovative sample preparation technique using focused ion beam (FIB) milling to fabricate micrometre-sized electron transparent lamellae that were then welded to the liquid cell substrate. This technique, for which we have described in detail all of the fabrication steps, allows for samples having dimensions of several square micrometres to be observed by TEM in situ in a liquid. We applied this technique to test whether we could observe and measure in situ dissolution of a crystalline material called wollastonite, a calcium silicate mineral. More specifically, this study was used to observe and record surface dynamics associated with step and terrace edge movement, which are ultimately linked to the overall rate of dissolution. The wollastonite lamella underwent chemical reactions in pure deionized water at ambient temperature in a liquid cell with a 5-math formulam-spacer thickness. The movement of surface steps and terraces was measured periodically over a period of almost 5 h. Quite unexpectedly, the one-dimensional rates of retreat of these surface features were not constant, but changed over time. In addition, there were noticeable quantitative differences in retreat rates as a function crystallographic orientation, indicating that surface retreat is anisotropic. Several bulk rates of dissolution were also determined (1.6–4.2 • 10 -7 mol m -2 s -1 ) using the rates of retreat of representative terraces and steps, and were found to be within one order of magnitude of dissolution rates in the literature based on aqueous chemistry data.

36 MATERIALS SCIENCE↗

Modelling and Optimization of Uranium (VI) Ions Adsorption Onto Nano-ZnO/Chitosan Bio-composite Beads with Response Surface Methodology (RSM)

Nano-ZnO-chitosan bio-composite beads were prepared for the sorption of UO{sub 2}{sup 2+} from aqueous media. The resulting nano-ZnO/CTS bio-composite beads were characterized by TEM, XRD etc. The sorption of UO{sub 2}{sup 2+} by bio-composite beads was optimized using RSM. The correlation between four variables was modelled and studied. According to RSM data, correlation coefficients (R{sup 2} = 0.99) and probability F-values (F = 2.24 × 10{sup − 10}) show that the model fits the experimental data well. Adsorption capacity for nano-ZnO/CTS bio-composite beads was obtained at 148.7 mg/g under optimum conditions. The results indicate that nano-ZnO/CTS bio-composite beads are appropriate for the adsorption of UO{sub 2}{sup 2+} ions from aqueous media. Also, the suitability of adsorption values to adsorption isotherms was researched and thermodynamic data were calculated.

77 NANOSCIENCE AND NANOTECHNOLOGY↗