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Recent reports of electron ptychography at atomic resolution have ushered in a new era of coherent diffractive imaging in the context of electron microscopy. We report and discuss electron ptychography under variable electron dose conditions, exploring the prospects of an approach which has considerable potential for imaging where low dose is needed.
A facile chemical process is described to produce graphene oxide utilizing a zwitterions amino acid intermediate from graphite oxide sheets. 11-aminoundecanoic acid molecules were protonated to intercalate molecules into the graphite oxide sheets to achieve ion exchange, and the carboxyl groups were then ionized in a NaOH solution to exfoliate the graphite oxide sheets. In this way, the produced graphene oxide nanosheets were stably dispersed in water. The delaminated graphene nanosheets were confirmed by XRD, AFM, and TEM. XRD patterns indicated the d{sub 002}-spacing of the graphite greatly increased from 0.380 nm and 0.870 nm. AFM and TEM images showed that the ordered graphite crystal structure of graphene nanosheets was effectively exfoliated by this method. The prepared graphene nanosheets films showed 87.1% transmittance and a sheet resistance of 2.1 Multiplication-Sign 10{sup 3} {Omega}/square. - Graphical abstract: A stable graphene oxide suspension could be quickly prepared by exfoliating a graphite oxide suspension by a host-guest electrostatic repulsion in aqueous solution. Highlights: Black-Right-Pointing-Pointer Graphene nanosheets were prepared by a zwitterions amino acid intermediate from graphite oxide. Black-Right-Pointing-Pointer 11-aminoundecanoic acid was protonated to intercalate molecules into the graphene oxide to achieve ion exchange. Black-Right-Pointing-Pointer The d{sub 002}-spacing of the graphite oxide greatly increased from 0.330 nm to 0.415 nm after 11-aminoundecanoic acid treatment.
The La{sub 0.75}Sr{sub 0.25}MnO{sub 3} (LSMO)/Ba{sub 0.7}Sr{sub 0.3}TiO{sub 3} (BSTO) superlattices and bilayers, where LSMO is ferromagnetic and BSTO is ferroelectric, were grown by dc sputtering. X-ray diffraction indicates that the samples present a textured growth with the c axis perpendicular to the substrate. Magnetization measurements show a decrease of the sample's magnetization for decreasing ferromagnetic thickness. This effect could be related to the presence of biaxial strain and a magnetic dead layer in the samples. Conductive atomic force microscopy indicates that the samples present a total covering of the ferromagnetic layer for a ferroelectric thickness higher than four unit cells. Transport tunneling of the carriers seems to be the preferred conduction mechanism through the ferroelectric layer. These are promising results for the development of multiferroic tunnel junctions.
Zn{sub 0.95}Mn{sub 0.05}O thin films were deposited on quartz substrates by radio-frequency magnetron sputtering using ceramic target in pure oxygen gas environment.. The X-ray diffraction and atomic force microscopy (AFM) studies reveal the nanocrysttalline nature of the films. The average grain size of the film is found to increase with increase in process gas pressure. The optical transmission spectra show the films to be highly transparent (80-95%).The direct energy band gap of film decreases from 3.04-2.92 eV with the increase in working gas pressure.
The growth of Ti{sub 3}SiC{sub 2} thin films were studied onto {alpha}-SiC substrates differently oriented by thermal annealing of TiAl layers deposited by magnetron sputtering. For any substrate's orientation, transmission electron microscopy coupled with x-ray diffraction showed the coherent epitaxial growth of Ti{sub 3}SiC{sub 2} films along basal planes of SiC. Specifically for the (1120) 4H-SiC, Ti{sub 3}SiC{sub 2} basal planes are found to be orthogonal to the surface. The continuous or textured nature of Ti{sub 3}SiC{sub 2} films does not depend of the SiC stacking sequence and is explained by a step-flow mechanism of growth mode. The ohmic character of the contact was confirmed by current-voltage measurements.
A new mixed surfactants system using alkyl carboxylic acids and quaternized poly[bis(2-chloroethyl)ether-alt-1,3-bis[3-(dimethylamino)propyl] urea] (PEPU) as the co-template was used to synthesize mesoporous silica materials with various morphologies and structures, including flakes, regular spheres, nanoparticles, and tube-spheres. The cationic polymer connected the anionic surfactant micelle to the anionic polysilicate species to induce the synthesis of the mesoporous silica materials. The structure and property of the surfactant and the cationic polymer determined the formation of mesoporous silica, and also had a signification influence on the morphology and structure of the final materials. To further explore the possible formation mechanism of these mesoporous materials, zeta potential was utilized to evaluate the interaction between the anionic surfactant and the cationic co-template. In addition, the structure, morphology, and porosity of these materials were characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and N{sub 2} adsorption-desorption measurements. - Graphical abstract: A new mixed surfactants system using alkyl carboxylic acids and PEPU as the co-template was used to synthesize mesoporous silica materials with various morphologies and structures. Highlights: {yields}A new mixed surfactants system induced the mesoporous silica materials with various morphologies and structure. > It is a development of the type S{sup -}N{sup +}I{sup -} route of the mesoporous formation. > Zeta potential was utilized to evaluate the interaction between the anionic surfactant and the cationic co-template. > The property and amount of surfactant and polymer determined the formation of the mesoporous materials.
The ammonia-based molecular beam epitaxy of GaN/(Al, Ga)N quantum dots is investigated using reflection high-energy electron diffraction, atomic force microscopy, transmission electron microscopy and photoluminescence. The main steps of the formation kinetics are identified and the influence of diffusion and evaporation processes on both the quantum dot and the wetting layer morphology is addressed. The correlation between the optical and structural properties of such structures finally allows for the analysis of matter exchanges between the quantum dots and the wetting layer during capping.
Porous {alpha}-Fe{sub 2}O{sub 3} hollow microspheres were synthesized through a simple and efficient carbon sphere template method. The samples were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy, transmission electron microscopy and N{sub 2} adsorption-desorption. Structural characterization indicated that as-prepared {alpha}-Fe{sub 2}O{sub 3} hollow microspheres had porous structure with around 200 nm in diameter and thin shell about 10 nm thick. The average pore size and Brunauer-Emmett-Teller specific surface area of {alpha}-Fe{sub 2}O{sub 3} hollow microspheres were 6.5 nm and 111.6 m{sup 2}/g, respectively. The gas sensing behavior investigation showed that as-synthesized {alpha}-Fe{sub 2}O{sub 3} hollow microspheres exhibited very good gas sensing property to acetone vapor. -- Graphical Abstract: HRTEM images of the {alpha}-Fe{sub 2}O{sub 3} hollow microspheres. Display Omitted
A simple, efficient and low-temperature approach for the assembly of hierarchical Zinc oxide (ZnO) microstructures in ionic liquid [EMIM]{sup +}[BF{sub 4}]{sup -} is reported. The as-obtained ZnO superstructures are composed of microbundles of nanorods from the center points, with the diameter and length in the range of 100-150 nm and 2-4 {mu}m, which have been characterized by X-ray diffraction, scanning and transmission electron microscopy, and photoluminescence spectroscopy. The ZnO microstructures exhibit significant defect-related green-yellow emission and high photodegradation of dye Methyl Orange (5x10{sup -5} mol/L) under UV excitation within 80 min. -- Graphical abstract: Easy formation of microbundles of ZnO nanorods were accomplished in low temperature with [EMIM]{sup +}[BF{sub 4}]{sup -} (1-ethyl-3-methylimidazolium tetrafluoroborate) ionic liquid, which exhibit significant green-yellow photoluminescence property and high photodegradation of Methyl Orange dye. Display Omitted Research highlights: {yields} Ionic liquid assisted solid-state route was introduced into synthesis of ZnO nanorods. {yields} The distinctive microbundles ZnO nanorod assembles was evidenced by SEM and TEM. {yields} ZnO nano-material exhibited high efficiency in photodegradation of Methyl Orange.
A simple route to selective decoration of nickel and nickel oxide nanocrystals on multiwalled carbon nanotubes (MWCNTs) using nickel acetylacetonate (NAA) was successfully achieved for the first time. The homogeneously decorated nanocrystals on MWCNTs were investigated for their structure and morphology by various techniques, such as powder X-ray diffraction, Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, transmission electron microscopy, field emission scanning electron microscopy and thermogravimetric analysis. It was found that the size distributions of the nanocrystals on MWCNTs ranged from 8 to 15 nm and they were well resolved. The precursor, NAA, was effectively employed to impregnate the MWCNTs, which on calcination at suitable temperatures and in the presence of hydrogen and nitrogen atmosphere gave rise to nickel and nickel oxide nanocrystals, respectively. -- Graphical abstract: Nickel and nickel oxide nanocrystals were selectively and homogeneously decorated on multiwalled carbon nanotubes using nickel acetylacetonate, as a precursor in a simple and efficient route. Display Omitted Highlights: {yields} A simple route for decoration of nickel and nickel oxide nanocrystals on MWCNTs. {yields} Nickel acetylacetonate used as nickel source for the first time to impregnate on MWCNTs. {yields} Selective decoration was achieved by calcination in hydrogen and nitrogen atmospheres. {yields} The as-decorated nickel and nickel oxide nanocrystals are in the range of 8-15 nm.
Structure determination of the fully intercalated phase Li{sub 12}Mo{sub 5}O{sub 17} and of the deintercalated oxide Li{sub 5}Mo{sub 5}O{sub 17} has been carried out by electron microscopy and neutron powder diffraction. The reversible topotactic transformation between the ordered rock salt structure of the former and the ribbon structure of the latter (closely related to that of Li{sub 4}Mo{sub 5}O{sub 17}) is explained on the following basis: both structures can be described as strips built up as an assembly of infinite ribbons of MoO{sub 6} octahedra that are five octahedra thick, and that differ by slight displacements of the octahedral ribbons. We show that the electrochemical behavior of the Li{sub x}Mo{sub 5}O{sub 17} system is based on two sorts of Li{sup +} sites; those that are located within the strips between the ribbons, and those that are located at the border of the strips. The high rate of Li intercalation in this oxide and its reversibility are discussed in terms of its peculiar structure. -- Graphical abstract: Structure determination of the fully intercalated phase Li{sub 12}Mo{sub 5}O{sub 17} and of the deintercalated oxide Li{sub 5}Mo{sub 5}O{sub 17} has been carried out by electron microscopy and neutron powder diffraction. The reversible topotactic transformation between the ordered rock salt structure of the former and the ribbon structure of the latter is explained on the following basis: both structures can be described as strips built up as an assembly of infinite ribbons of MoO{sub 6} octahedra that are five octahedra thick, and that differ by slight displacements of the octahedral ribbons. We show that the electrochemical behavior of the Li{sub x}Mo{sub 5}O{sub 17} system is based on two sorts of Li{sup +} sites; those that are located within the strips between the ribbons, and those that are located at the border of the strips. The high rate of Li intercalation in this oxide and its reversibility are discussed in terms of its peculiar structure. Research highlights: {yields} Electron microscopy and neutron powder diffraction structure determination {yields} We have explained the reversible topotactic transformation between an ordered rock salt structure and a ribbon structure {yields} We show that the electrochemical behavior of the Li{sub x}Mo{sub 5}O{sub 17} system is based on two sorts of Li{sup +} sites {yields} The high rate of Li intercalation in this oxide and its reversibility are discussed in terms of its peculiar structure.
Lithium metasilicate (Li{sub 2}SiO{sub 3}) was successfully synthesized using a hydrothermal process in the presence of different surfactants with cationic, non-ionic and anionic characters. The samples obtained were compared to a sample prepared by the conventional solid-state reaction method. The structural and microstructural characterizations of different Li{sub 2}SiO{sub 3} powders were performed using various techniques. Diffraction analyses revealed the successful crystallization of pure Li{sub 2}SiO{sub 3} single phase by hydrothermal technique, even without further heat-treatments and independent of the surfactant used. Electron microscopy analyses revealed that Li{sub 2}SiO{sub 3} powders were composed of uniform micrometric particles with a hollow sphere morphology and nanostructured walls. Finally, different thermal analyses showed that Li{sub 2}SiO{sub 3} samples preserved their structure and microstructure after further thermal treatments. Specific aspects regarding the formation mechanism of the spherical aggregates under hydrothermal conditions are discussed, and there is a special emphasis on the effect of the synthesis pathway on the morphological characteristics. -- Graphical abstract: Li{sub 2}SiO{sub 3} was synthesized using a hydrothermal process in the presence of different surfactants. Li{sub 2}SiO{sub 3} powders were composed of uniform micrometric particles with a hollow sphere morphology and nanostructured walls. Display Omitted Highlights: {yields} Pure Li{sub 2}SiO{sub 3} was synthesized by the hydrothermal method. {yields} Surfactant addition produced microstructural and morphological variations. {yields} TEM reveled the generation of nanostructured hollow spheres.
Solvothermal synthesis is an efficient synthetic method for preparing nano and micromaterials. Preparation of hematite through alcoholysis of ferric ion under solvothermal condition has been carried out at low concentrations. In this paper, Fe{sub 2}O{sub 3} homogeneous core/shell hierarchical nanostructures were synthesized via solvothermal treatment of FeCl{sub 3}{center_dot}6H{sub 2}O and ethanol. The achievements of such structures can be attributed to two important factors: high temperature and high concentration. Besides, the crystal water and reaction time were also important factors to the synthesis of hematite. The prepared samples were characterized using X-ray powder diffraction, Raman spectra, scanning electron microscopy equipped with an energy-dispersive X-ray spectrometer, transmission electron microscopy and Brunauer-Emmett-Teller surface area and pore size distribution. X-ray photoelectron spectroscopy showed a satellite peak at 719.8 eV, which is the characteristic peak of Fe(III). The formation mechanism of the spheres and the effects of the reactant concentrations and reaction temperatures have been discussed. Moreover, the enhanced catalytic activity of the spheres has also been investigated through oxidation of benzyl alcohol to benzaldehyde with high conversion (42%) and selectivity (95%). - Graphical abstract: Fe{sub 2}O{sub 3} homogeneous core/shell hierarchical microspheres were synthesized by solvothermal method. Owing to the special structure, the synthesized Fe{sub 2}O{sub 3} microspheres exhibit a superior catalytic activity in benzyl oxidation. Highlights: Black-Right-Pointing-Pointer Hierarchical Fe{sub 2}O{sub 3} core/shell microspheres were synthesized. Black-Right-Pointing-Pointer Microspheres were assembled by {beta}-FeOOH. Black-Right-Pointing-Pointer The sample exhibits a superior catalytic activity and selectivity. Black-Right-Pointing-Pointer The high activity and selectivity are due to the hierarchical core/shell structure.
CdS thin films on LiNbO{sub 3} (1 0 4) and silicon (1 1 1) substrates were prepared through an atom substitution technique using cadmium nitrate as a reactant in an H{sub 2}S atmosphere at 230 {sup o}C. X-ray diffraction, scanning electron microscopy and transmission microscopy results indicate that the CdS film grows on LiNbO{sub 3} oriented along the [0 0 1] axis in form of crystallized nanoplates, while that deposited on silicon forms randomly oriented nanoparticles. Investigation of the precursor thin film suggests that CdS forms from the O in the CdO precursor thin film being substituted by S from H{sub 2}S in the surrounding environment, which is designated as an atom substitution process. This novel method involving an atom substitution reaction between the CdO precursor thin film and its environment can provide a new low cost approach to the preparation of chalcogenide or other compound thin films. A schematic illustration and corresponding mechanism describing the details of this method are proposed. -- Graphical abstract: Elemental O in CdO is substituted by elemental S from the atmosphere in the apparatus, which is designated as an atom substitution process. This novel method involving an atom substitution reaction between the CdO precursor thin film and its environment can provide a new low cost approach to the preparation of chalcogenide or other compound thin films. Display Omitted Research highlights: {yields} An atom substitution method for thin film preparation was demonstrated. {yields} Combination of the atom substitution and spin coating method was achieved. {yields} Well oriented CdS thin film was prepared on LiNbO{sub 3} substrate. {yields} The atom substitution method could be used for many compound systems.
Perovskite-type KTaO{sub 3} powder was synthesized by an alternative solid-state method at low temperature. Stoichiometric ammonium tantalum hydroxide, K{sub 2}C{sub 2}O{sub 4} and KF were mixed in water and then dried at room temperature. The crude product was formed by calcining the dried mixture at different temperatures. Pyrochlore-free KTaO{sub 3} powder was successfully synthesized after treating the crude product with water. KF plays an important role to inhibit the formation of pyrochlore K{sub 2}Ta{sub 2}O{sub 6} during the calcination process of ammonium tantalum hydroxide/K{sub 2}C{sub 2}O{sub 4}/KF mixture. X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier-transform infrared (FTIR) spectroscopy, UV-vis diffuse reflectance (UV-vis) spectroscopy and thermogravimetric (TG) analysis were used to characterize the precursor compound and as-prepared samples. XRD results show that pyrochlore-free KTaO{sub 3} powder can be obtained at 600 deg. C. SEM results reveal that the as-prepared products are agglomerated and each of the agglomerations consists of many small grains with 10-30 nm in diameter. - Graphical abstract: Pyrochlore-free KTaO{sub 3} powder was prepared at 600 deg. C using tantalum hydroxide/K{sub 2}C{sub 2}O{sub 4}/KF raw materials. Pyrochlore K{sub 2}Ta{sub 2}O{sub 6} and perovskite KTaO{sub 3} coexist at 600 deg. C using tantalum hydroxide/K{sub 2}C{sub 2}O{sub 4} raw materials. Highlights: > In-situ degradation of TaO{sub x}(OH){sub 5-x}(NH{sub 4}){sub x}, K{sub 2}C{sub 2}O{sub 4} and KF promotes the reaction. > Synthesis of KTaO{sub 3} displayed a two-step reaction path with the intermediate formation of K{sub 2}TaO{sub 3}F. > Formation of intermediate K{sub 2}TaO{sub 3}F benefits to prepare pyrochlore-free KTaO{sub 3} at low temperature. > Pyrochlore-free KTaO{sub 3} is prepared at 600 deg. C, which is the lowest temperature reported so far by hard chemistry method. > Synthetic method is a facile, rapid, low price and environment friendly route.
Bragg coherent diffractive imaging (BCDI) is a non-invasive microscopy technique that can visualize the morphology and internal lattice deviations of crystals with nanoscale spatial resolution and picometer deformation sensitivity. While BCDI has been successfully applied in various studies of materials, it is less successful for highly-strained crystals. Specifically, it is difficult to correctly reconstruct the electron density of a highly-strained object using conventional phase retrieval algorithms. Although various algorithms have been developed to overcome this challenge, most of them require a priori knowledge that is not always available in practice. Here we report on a new phase retrieval workflow that can invert diffraction patterns from multiple Bragg peaks simultaneously. The new workflow is explored via simulated diffraction from crystals with various strain conditions. Furthermore, reconstructions from the new workflow consistently demonstrate more accurate electron density maps, in comparison with the conventional method. For highly-strained crystals, the new workflow improves the reliability and consistency of BCDI phase retrieval significantly.
Single-phase {alpha}-MnO{sub 2} nanorods and {delta}-MnO{sub 2} nano-fiber clumps were synthesized using manganese pentahydrate in an aqueous solution. These nanomaterials were characterized using the Transmission Electron Microscope (TEM), Field Emission Scanning Electron Microscope (FE-SEM), Powder X-ray diffraction (XRD) and the Brunauer-Elmet-Teller nitrogen adsorption technique (BET-N{sub 2} adsorption). The structural analysis shows that {alpha}-MnO{sub 2} (2x2 tunnel structure) has the form of needle-shaped nanorods and {delta}-MnO{sub 2} (2D-layered structure) consists of fine needle-like fibers arranged in ball-like aggregates. Batch adsorption experiments were carried out to determine the effect of pH on adsorption kinetics and adsorption capacity for the removal of As(V) from aqueous solution onto these two types of nanoadsorbents. The adsorption capacity of As(V) was found to be highly pH dependent. The adsorption of As(V) onto {alpha}-MnO{sub 2} reached equilibrium more rapidly with higher adsorption capacity compared to {delta}-MnO{sub 2}. -- Graphical abstract: {alpha}-MnO{sub 2} (2x2 tunnel structure) nanorods and {delta}-MnO{sub 2} (2-D layered structure) nano-fiber clumps were synthesized in a facile way in an aqueous solution and characterized by TEM, FE-SEM, XRD and BET-N{sub 2} adsorption techniques. The structural analysis shows that {alpha}-MnO{sub 2} is needle shaped nanorods and {delta}-MnO{sub 2} consists of 2-D platelets of fine needle-like fibers arranged in ball-like aggregates. Further batch experiments confirmed that both nanoadsorbents are potential candidates for the adsorption of As(V) with a capacity of 19.41 and 15.33 mg g{sup -1} for {alpha}-MnO{sub 2} and {delta}-MnO{sub 2}, respectively. The presence of As3d peak in XPS study indicates that arsenic on the surface of nanoadsorbents is in the stable form of As(V) with a percentage of arsenate onto {alpha}-MnO{sub 2} is 0.099% as compared to 0.021% onto {delta}-MnO{sub 2}, clearly indicating the higher adsorption of As(V) in case of {alpha}-MnO{sub 2} as compared to {delta}-MnO{sub 2}, which is in good agreement with the adsorption studies results. Display Omitted
The anticancerous drug methotrexate (MTX) has been intercalated into an ZnAl-layered double hydroxide (LDH) using an anion exchange technique to produce LDH-MTX hybrids having particle sizes in the range of 100-300 nm. X-ray diffraction studies revealed increases in the basal spacings of ZnAl-LDH-MTX hybrid on MTX intercalation. This was corroborated by the transmission electron micrographs, which showed an increase in average interlayer spacing from 8.9 A in pristine LDH to 21.3 A in LDH-MTX hybrid. Thermogravimetric analyses showed an increase in the decomposition temperature for the MTX molecule in the LDH-MTX hybrid indicating enhanced thermal stability of the drug molecule in the LDH nanovehicle. The cumulative release profile of MTX from ZnAl-LDH-MTX hybrids in phosphate buffer saline (PBS) at pH 7.4 was successfully sustained for 48 h following Rigter-Peppas model release kinetics via diffusion. - Graphical abstract: ZnAl-layered double hydroxide intercalated with methotrexate ({approx}34% loading) promises the possibility of use of ZnAl-LDH material as drug carrier and in controlled delivery. Highlights: > ZnAl-layered double hydroxide methotrexate nanohybrid has been synthesized. > XRD and TEM studies on nanohybrid revealed successful intercalation of methotrexate. > TG and CHN analyses showed {approx}34 wt% of methotrexate loading into the nanohybrid. > Possibility of use of ZnAl-LDH material as drug carrier and in delivery.