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X-ray powder diffraction data, unit-cell parameters, and space group for inclusion complex of β-cyclodextrin with fraxinellone, C42H70O35·C14H16O3·3H2O, are reported [a = 19.294(2) Å, b = 26.639(1) Å, c = 16.467(3) Å, β = 110.451(9)°, cell volume V = 7930.34 Å3, Z = 4 and space group C2]. All measured lines were indexed and are consistent with the C2 space group. No detectable impurities were observed.
We present a quantitative in-situ transmission electron microscope (TEM) study of stress-assisted grain growth in 75 nm thick platinum thin films. We utilized notch-induced stress concentration to observe the microstructural evolution in real time. From quantitative measurements, we find that rapid grain growth occurred above 290 MPa of far field stress and ~0.14% elongation. This value is found to be higher than that required for stable interface motion but lower than the stress required for unstable grain boundary motion. We attribute such grain growth to geometrical incompatibility arising out of crystallographic misorientation in adjoining grains, or in other words, geometrically necessary grain growth.
The strain-rate sensitivity of ultrafine-grained aluminum (Al) and nanocrystalline nickel (Ni) is studied with an improved nanoindentation creep method. Using the dynamic contact stiffness thermal drift influences can be minimized and reliable creep data can be obtained from nanoindentation creep experiments even at enhanced temperatures and up to 10 h. For face-centered cubic (fcc) metals it was found that the creep behavior is strongly influenced by the microstructure, as nanocrystalline (nc) as well as ultrafine-grained (ufg) samples show lower stress exponents when compared with their coarse-grained (cg) counterparts. The indentation creep behavior resembles a power-law behavior with stress exponents n being ∼ 20 at room temperature. For higher temperatures the stress exponents of ufg-Al and nc-Ni decrease down to n ∼ 5. These locally determined stress exponents are similar to the macroscopic exponents, indicating that similar deformation mechanisms are acting during indentation and macroscopic deformation. Grain boundary sliding found around the residual indentations is related to the motion of unconstrained surface grains.
The hardness changes caused by formation of the metastable and stable phases were examined and correlated with the microstructural changes in grain interior and grain boundary during aging at 350 °C to clarify the age-hardening and softening mechanism of a low-gold Au-Cu-Ag-Pd dental alloy. Aging in this context refers to the time-delay that occurs wherein such alloys are kept at elevated temperatures for periods upto many hours to allow precipitation or ordering to take place. During the period of increasing hardness, the matrix was separated into the Ag-rich α1 and AuCu I phases through the metastable phases, forming block-like structure. The apparent hardening was attributed primarily to lattice strain due to the tetragonality of AuCu I′ [the primer (′) here indicates a metastable phase; likewise (I) and (I′) indicate stable AuCu I and metastable AuCu I′ phases, respectively] and AuCu I phases along the c-axis, secondarily to the coherency or semicoherency strain between the metastable α1′ and AuCu I′ phases and between the α0 and AuCu I phases along the a-axis. The apparent softening was caused primarily by growth and coarsening of the lamellar structure in the grain boundaries, secondarily by coarsening of the block-like structure in the grain interior.
Ni–base alloy coatings were fabricated on 45 steel by laser cladding using a CW-CO2 laser system. The microstructure of the coatings was analyzed using optical microscope (OM), scanning electronic microscope (SEM), and x-ray diffractometer (XRD). The phase fractions, phase compositions, and solidification process in the coatings were calculated using Thermo-Calc software and compared with experimental results. The results show that a dense crack- and porous-free coating with good metallurgical bond is obtained under optimal process parameters. The coatings can be divided into three regions: clad zone (CZ), bonding zone, and heat-affected zone of the substrate. The CZ consists of γ-Ni, M7C3, CrB, and Ni3B phases. Based on the calculated results, the solidification process and reaction scheme in the coatings were discussed. The calculated results obtained from Thermo-Calc software agree with the experimental data well. It is beneficial to the coating design for a desirable microstructure and mechanical properties.
A quasicrystal (QC)- based alloy composite was made by copper mold casting under a low-vacuum level condition at the bulk metallic glass (BMG)- forming composition (Zr65Cu15Al10Ni10)90Nb10. The QC alloy consisted of a majority of icosahedral quasicrystal phase and a small amount Zr-rich glassy phase. Under uniaxial compression at room temperature, the BMG alloy exhibits a certain plastic strain; the QC alloy is much stronger but brittle. The icosahedral glass model was used to describe the I-phase structure. The structure–property relations of the BMG and QC alloys are discussed assuming the common preferential icosahedral atomic structure in both cases and the existence of local glue structure in the BMG structure.
A simple and modified solvothermal method using oxalate precursor, used to synthesize Cd1−xNixO (x = 0.047, 0.102, and 0.163) nanoparticles and their phase structure, morphology, optical and magnetic properties, have been investigated. X-ray diffraction studies revealed that as-prepared Ni-doped CdO solid solutions are highly crystalline and stabilized in a monophasic cubic CdO structure. X-ray diffraction and ICP-MS studies confirmed the incorporation of Ni2+ in a CdO matrix. The average grain size was found to be 30, 15, and 11 nm, respectively, using transmission electron microscopic studies. High surface area in the range of 118–143 m2/g has been achieved for these solid solutions using the multipoint BET method, which increases on increasing Ni concentration in Cd lattice site. The optical band gap of these solid solutions shows red shift to the undoped CdO. Ni-doped CdO nanoparticles exhibit co-existence of paramagnetism and ferromagnetism.
Sn–40 at.% Mn peritectic alloys were directionally solidified at different growth rates (1–100 μm/s) under a steep temperature gradient (40 K/mm). The migration of secondary dendrite arm was observed in this peritectic alloy in which both the primary phase and the peritectic phase are intermetallic compounds with nil solubility. This migration is caused by coupling remelting/solidification at the hot/cold sides of the liquid pool between two adjacent secondary dendrite arms by temperature gradient zone melting. Its novel feature is that the remelting temperature of primary phase is a little higher than the solidification temperature of peritectic phase. Analytical solutions based on the assumption that the solubility of both primary and peritectic phases are nil have been proposed to describe this migration. It has also been found that the migration of secondary dendrite arm is most obvious at intermediate growth rates under steep temperature gradient in the directionally solidified Sn–40 at.% Mn peritectic alloy.
Self-assembled nanostructures often exhibit unique properties that are distinct from those of bulk materials. During the past decade, significant progress has been made in the assembly of nanorods and understanding some of the self-directing assembly mechanisms, particularly related to gold nanorods. Nonetheless, methods that can be scaled up to large areas for device-scale applications are yet to be established. This review describes various routes that are being actively pursued to achieve assembly of nanorods. Self-assembly methods that utilize external forces such as electric field or gravitational forces are reviewed. Additionally, self-assembly schemes using chemical and biomolecule linkers are presented. Other important routes, such as template assisted assembly, Langmuir-Blodgett, and nanorod assembly methods carried out in solution phase are also discussed. The latter includes recently reported approaches to produce superstructured particles through self-assembly. Solvent evaporation and drying can also strongly contribute to the assembly of nanostructures. The final section presents self-assembly routes that primarily exploit the drying kinetics of solvents.
Zinc oxide (ZnO)–single-walled carbon nanotubes (SWCNTs) nanocomposite thin films have been grown by chemical bath deposition method. The changes in structural and chemical properties were studied by means of x-ray diffraction, field-emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM) and Fourier transform infrared spectroscopy (FTIR). The average crystallite size of ZnO doped with 0.1 and 0.5 wt% SWCNTs was measured about 14.69 and 17.76 nm, respectively. Texture coefficient of the carbon peak (002) was investigated as more than 3.2995 for ZnO mixed with 0.5 wt% SWCNTs. SEM images revealed the ZnO and SWCNTs entangled between the particles. TEM images estimated the inner and outer diameters of SWCNTs to be about 4.86 and 11.32 nm, respectively. FTIR analysis proved the formation of Zn–O and C bonding in the thin films. The performance of the dye-sensitized solar cells (DSSCs) was found to depend on the loading of SWCNTs. The power conversion efficiency increased from 0.078 to 0.684% after loading with 0.1 wt% SWCNTs. Higher amount of SWCNTs (0.5 wt%) was determined as ineffective in improving the performance of ZnO-based DSSCs.
In this study, we are reporting the time- and temperature-dependence of the electrical resistivity and temperature-dependence of the Hall voltage in neodymium nickelate thin films. The films were deposited on a lanthanum aluminate substrate [LaAlO3 (001)] by a pulsed laser deposition technique, with thicknesses ranging from 0.6 to 120 nm. Time-dependent electrical transport measurements indicated the formation of a kinetically stable metallic glassy phase rather than a stable insulating phase on cooling below the transition temperature, TM-I. Comparisons of the low-temperature behavior with that of common insulators further supported this claim. Hall effect measurements on the 1.2-nm sample showed a local maximum in the carrier concentration just below the TM-I on both the heating and cooling cycles. This again confirmed the proposed low-temperature structure, in that, for the 1.2-nm sample, there was a minimal degree of supercooling before transitioning to a kinetically stable glassy phase.
In the present study, aminofunctionalized mesoporous silica (AFMS) was synthesized using the anionic surfactant N-lauroylsarcosine sodium as template and 3-aminopropyltrimethoxysilane as costructure directing agent. The synthesized mesoporous silica was characterized by the Fourier transform infrared spectra, x-ray diffraction, N2 adsorption-desorption, scanning electron microscopy, and transmission electron microscopy techniques. The application for the removal of Ni2+ from aqueous solution using the synthesized mesoporous silica as adsorbent was investigated. It was found that the solution pH affected adsorption of Ni2+ greatly. The kinetic data of adsorption showed that the removal rate of Ni2+ was substantially high. The adsorption isotherms were fitted using the Sips, Langmuir, and Freundlich models, respectively, and the results showed that the Sips model was the best one to describe the experimental data. From the data of Sips, the maximum adsorption capacity of Ni2+ in respect of the extracted sample is 2.48 mmol/g, much higher than those reported in other literature. The possible adsorption mechanism of Ni2+ on the AFMS was proposed.
We examine the development of stable bimetal interfaces in nanolayered composites in severe plastic deformation. Copper-niobium multilayers of varying layer thicknesses from several micrometers to 10 nanometers (nm) were fabricated via accumulative roll bonding (ARB). Investigation of their 5-parameter character and atomic scale structure finds that when layer thicknesses refine well below one micrometer, the interfaces self-organize to a few interface orientation relationships. With atomic scale and crystal plasticity modeling, we identify that the two controlling factors that determine whether an interface is stable under high strain rolling are orientation stability of the bicrystal and interface formation energy. A figure-of-merit is introduced that not only predicts the development of the prevailing interfaces but also explains why other interfaces did not develop. Through a suite of nanomechanical and bulk test results, we show that ARB composites containing these stable interfaces are found to have exceptional hardness (∼4.5 GPa) and strength (∼2 GPa).
The organic light-emitting (OLE) materials have attracted great interest due to their potential applications in sensors, biodetectors and OLE devices. However, highly efficient emission from organic solids is still a great challenge because of the aggregation-caused quenching effect. In this article, a three-dimensional (3D) organic-inorganic hybrid nanoparticle, based on polyhedral oligomeric silsesquioxane (POSS), was precisely fabricated via click chemistry with high yield, and its structure was characterized by Fourier transform infrared spectroscopy, 1H, and 29Si nuclear magnetic resonance spectroscopies, and Matrix-Assisted Laser Desorption Ionization Time-of-Flight Mass Spectrometry, respectively. The resultant 3D organic-inorganic nanohybrid showed significantly enhanced emission in solid film (Φfilm 80%) with a slight red-shift as compared with its organic counterpart, (Φfilm 14%), which exhibits a large red-shift in solid film, due to the deaggregation effect of POSS. Simultaneously, the resultant nanohybrid also exhibited good film formability, excellent spectrum and thermal stability (>250 °C) due to the introduction of POSS.
This complete, yet concise, guide introduces you to the rapidly developing field of high throughput screening of biomaterials: materiomics. Bringing together the key concepts and methodologies used to determine biomaterial properties, you will understand the adaptation and application of materomics in areas such as rapid prototyping, lithography and combinatorial chemistry. Each chapter is written by internationally renowned experts, and includes tutorial paragraphs on topics such as biomaterial-banking, imaging, assay development, translational aspects, and informatics. Case studies of state-of-the-art experiments provide illustrative examples, whilst lists of key publications allow you to easily read up on the most relevant background material. Whether you are a professional scientist in industry, a student or a researcher, this book is not to be missed if you are interested in the latest developments in biomaterials research.
The microstructure evolution and mechanical responses are investigated in uniaxial tensile test performed on AZ31 magnesium alloy sheets processed by the flat extrusion container. A novel emphasis based on the texture was used to estimate the relative magnitude of hardening effects related to the deformation twinning. The anisotropic behavior of the sheets is sensitive to the orientation of the crystals with respect to the loading direction. This is ascribed to the effect of the initial texture and the activation of their relative critical resolved shear stresses on slip and twinning. The increased accumulated hardening increases the twin nucleation stress. The deformation twinning significantly induces an asymmetry in the yield behavior. Moreover, it remarkably prolongs the slope of the stage II in the working hardening curve. An accepted notion is proposed that the preferential activity of deformation twinning exerts a significant effect on mechanical anisotropy during tension.
The fast dissolution of certain calcium-containing compounds makes them attractive carriers for trace minerals in nutritional applications, e.g., iron and zinc to alleviate mineral deficiencies in affected people. Here, CaO-based nanostructured mixed oxides containing nutritionally relevant amounts of Fe, Zn, Cu, and Mn were produced by one-step flame spray pyrolysis. The compounds were characterized by nitrogen adsorption, x-ray diffraction, (scanning) transmission electron microscopy, and thermogravimetric analysis. Dissolution in dilute acid (i.d.a.) was measured as an indicator of their in vivo bioavailability. High contents of calcium resulted in matrix encapsulation of iron and zinc preventing formation of poorly soluble oxides. For 3.6 ≤ Ca:Fe ≤ 10.8, Ca2Fe2O5 coexisted with CaO. For Ca/Zn compounds, no mixed oxides were obtained, indicating that the Ca/Zn composition can be tuned without affecting their solubility i.d.a. Aging under ambient conditions up to 225 days transformed CaO to CaCO3 without affecting iron solubility i.d.a. Furthermore, Cu and Mn could be readily incorporated in the nanostructured CaO matrix. All such compounds dissolved rapidly and completely i.d.a., suggesting good in vivo bioavailability.