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At least 613 records · Page 34

Sparse modeling of space- and time-varying diffraction response of a progressively loaded aluminum alloy

Highlights: • Plasticity induces crystal orientation and lattice spacing heterogeneity. • High energy x-ray diffraction spot broadening typically accompanies plasticity. • Method quantifies spot broadening in difficult, mixed microstructure data. • Algorithm finds sparse combination of entries from dictionary of peak functions. • Approach showed asymmetric plastic response in preprocessed AA7075 T651 sample. - Abstract: High energy X-ray diffraction data collected in situ during loading experiments permits probing of the crystal structure of a plastically deforming material sample. An elastoplastic deformation is associated with heterogeneity in both crystal orientation and lattice spacing—each manifesting as azimuthal broadening and radial broadening of diffraction peaks respectively. Quantifying the spreading effect is challenging, especially in cases where the sample has a granularity between that of a single crystal and fine grain or powder material. The approach developed in this paper begins by modeling the intensity signal in the vicinity of a Debye-Scherrer ring as a sparse, nonnegative superposition of Gaussian basis functions drawn from an over-complete dictionary. Processing automatically selects from the dictionary basis functions whose widths and amplitudes are representative of the data. The chosen basis functions are used to compute scalar measures of radial and azimuthal broadening for the set of diffraction peaks composing a Debye-Scherrer ring. To demonstrate the utility of the approach, we show that analysis of diffraction peak shape information from an aluminum alloy 7075 T651 (AA7075 T651) sample provides insight into the origin of material state that would have otherwise have been difficult if not impossible to extract using conventional methods. Furthermore, the extracted information revealed a deformation response linked to the processing history of the sample.

36 MATERIALS SCIENCE↗

Free surface effects on the recrystallization of compressed, stable, Al-Mn single crystals

Highlights: • The free surface provokes high frequency nucleation. • The free surface and surface ‘quality’ do not modify the orientations of the recrystallized grains. • The misorientation relations across recrystallization front are similar for all sections of both orientations. The free surface effect on the grain crystallography and morphology during recrystallization has been studied in stable Goss {110}001 and brass {110}112 - oriented single crystals of Al-1%wt.Mn alloy. The samples were plane strain compressed up to a strain of about 0.5 to develop a homogeneous structure comprising two sets of symmetrical microbands and then lightly annealed. The variation of recrystallization after annealing was then analysed by optical microscopy and SEM/EBSD on different cross-sections. The results are discussed in terms of the misorientation angle and axis distributions. The free surface provokes high frequency nucleation leading to a small grain size compared to internal sections of the bulk sample. However, the free surface and surface ‘quality’ do not modify the orientations of the recrystallized grains, i.e. similar groups of recrystallized grain orientations were observed for all sections. This leads to a strong misorientation relation between deformed/recovered area orientations and the limited number of groups of recrystallized grain orientations, basically the same as those observed during bulk recrystallization of similar crystals.

36 MATERIALS SCIENCE↗

Crystal rotation and microstructures in an aluminum single-slip system under tensile loading

Highlights: • The crystal rotation angle with the progression of ductile damage was larger in the vertical plane than that in the horizontal plane. In the measurement along 110, the relative rotation angle was the maximum at the intersection of 111 and 110. • The integrated intensity and the FWHM decreased near the notch (from 0 to 0.3 mm) as well as at the intersection of 110 and 111 in the measurement along 110. • The dislocation cell size and the dislocation density decreased at the intersection of 111 and 110 in the measurement of 110 for ε = 5%. This behavior was attributed to the strain energy being released by the rotation of the dislocation cell. We experimentally investigated the rotation angle of the (220) plane in an aluminum single-slip system in which the angles of 110 and 111 in the single crystal were 45° relative to the tensile loading direction. Crystal rotation was investigated at several spots (50 × 50 μm) along 110 and 111 using synchrotron radiation white X-rays at the BL28B2 beamline of super photon ring-8. In measurements along the 110 axis, at an applied strain of ε = 5%, the relative crystal rotation of (220) in the vertical plane increased from 0.850° to 5.438° in the range of 0.9 to 1.4 mm. We observed the microstructure using a transmission electron microscope and verified the size of the dislocation cells or subgrains at each spot along 110. The fundamental local crystallography revealed in this work should be helpful in establishing a method for evaluating ductile damage in materials.

36 MATERIALS SCIENCE↗

Single crystalline β-Ga{sub 2}O{sub 3} nanowires synthesized by thermal oxidation of GaSe layer

Highlights: ► β-Ga{sub 2}O{sub 3} nanowires were synthesized through annealing GaSe crystal. ► Nanowires obtained at different annealing temperatures were characterized. ► A possible growth mechanism was proposed. - Abstract: β-Ga{sub 2}O{sub 3} nanowires were grown by thermal oxidation of GaSe single crystal surface under a mixture of argon–air flow, without the presence of a catalyst or foreign substrate. The nanowires were obtained after annealing GaSe surface at different temperatures (720 °C, 850 °C and 930 °C) for 5 h and they were characterized by X-ray diffraction, Raman spectroscopy, scanning electron microscopy, transmission electron microscopy and selected area diffraction pattern. The lengths of the nanowires varied in the range 50–180 nm, while the typical diameters of the nanowires were in the range 60–90 nm. A possible mechanism has been proposed in order to explain the growth of oxide nanowires.

36 MATERIALS SCIENCE↗

Water induced size and structure phase transition of CdS crystals and their photocatalytic property

Graphical abstract: Excellent photocatalytic activity in degradation of RhB was found with the hexagonal CdS nanorods growing along [0 0 0 1] direction, which is a result of the exposed (0 0 0 1) facets in the ends. Display Omitted Highlights: ► CdS microwires and nanorods were attained by a modified CHM approach. ► The phase transition (cubic to hexagonal) was achieved by tuning the amount of H{sub 2}O. ► Excellent photocatalytic activity was found with the hexagonal CdS. ► Hexagonal CdS has the better catalytic property due to more (0 0 0 1) facets exposed. -- Abstract: Single-crystalline CdS microwires (mixed cubic and hexagonal phase) and nanorods (pure hexagonal phase) were synthesized by a modified composite-hydroxide-mediated (CHM) approach. Photocatalytic degradation of rhodamine B with the CdS nanorods was studied under the simulated sunlight irradiation. Crystalline phase transition from cubic to hexagonal phase was achieved by adding a small amount of water in the melts. The phase structures and morphologies of the prepared products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), selected area of electron diffraction (SAED) and scanning electron microscopy (SEM), respectively. The results show that the pure hexagonal phase structure could be obtained with 5 mL or more than 5 mL water added in the composite-hydroxide melts. The band–gap of the hexagonal nanorods was 2.435 eV observed from UV–vis reflection spectrum. Compared with the CdS nanoparticles (mixed cubic and hexagonal phase), we found that the hexagonal phase structure CdS nanorods revealed much better photocatalytic activity owing to the exposure of (0 0 0 1) polar facet on the end. It is expected that the present research may offer useful guidance to the potential application of CdS in the treatment of environmental pollution.

36 MATERIALS SCIENCE↗

CdB{sub 10}O{sub 14}(OH){sub 4}·H{sub 2}O with an unprecedented decaborate fundamental building block

Graphical abstract: Display Omitted Highlights: ► CdB{sub 10}O{sub 14}(OH){sub 4}·H{sub 2}O is prepared by boric acid flux method. ► Its structure is solved by single-crystal X-ray diffraction in space group P2{sub 1}/n. ► It possesses an unprecedented decaborate fundamental building block B{sub 10}O{sub 20}. ► Structure features are discussed in detail and compared with other polyborates. -- Abstract: CdB{sub 10}O{sub 14}(OH){sub 4}·H{sub 2}O has been synthesized under boric acid flux condition and characterized by single-crystal X-ray diffraction, infrared spectra, and UV–vis reflectance spectroscopy. It crystallizes in the monoclinic space group P2{sub 1}/n with a = 7.7277(8), b = 18.95(2), c = 9.8616(10) Å, β= 91.454(1)°, V = 1443.7(3) Å. The structure consists of [B{sub 10}O{sub 16}(OH){sub 4}] layers of 9-membered borate rings enclosing Cd{sup 2+} cations. Adjacent borate layers are interconnected via hydrogen bonding to form a 3D network. It possesses an unprecedented decaborate fundamental building block B{sub 10}O{sub 20}. The structure details are discussed together with Sr[B{sub 6}O{sub 9}(OH){sub 2}]·3H{sub 2}O, Pb[B{sub 8}O{sub 11}(OH){sub 4}], Pr[B{sub 8}O{sub 11}(OH){sub 5}], and Nd[B{sub 9}O{sub 13}(OH){sub 4}]·H{sub 2}O, which have correlated FBBs. The band structure calculations show its direct energy band gap of ∼4.68 eV, in consistent with the estimated value (4.77 eV) from UV–vis. In addition, dielectric constants and refractive indexes are also calculated.

36 MATERIALS SCIENCE↗

A simple and fast preparation of neodymium-substituted nanocrystalline Mn{sub 2}O{sub 3}

Graphical abstract: Synthesis of Mn{sub 2−x}Nd{sub x}O{sub 3} with mixed morphology -- Abstract: Neodymium (Nd) ions were substituted for manganese in the crystal lattice of synthetic Mn{sub 2}O{sub 3}, via oxidation of Mn(NO{sub 3}){sub 2} in basic solution at room temperature. Doping of Nd into the lattice structure of Mn{sub 2}O{sub 3} has been reported for the first time, which resulted in materials with new composition, morphology and optical properties. The synthesized materials were characterized by XRD, SEM, TEM, HRTEM, XPS and TOF-SIMS. Light (2.6%) Nd doping resulted in a mixture of rods, plates and small sheets, while heavy (8.9%) Nd doping resulted in rods, large sheets and large single crystals. The effect of structural doping of Nd ions into Mn{sub 2}O{sub 3} resulted in a red shift in the absorbance.

36 MATERIALS SCIENCE↗

Structure and luminescence properties of thermally nitrided Ga{sub 2}O{sub 3} nanowires

Graphical abstract: The as-synthesized Ga{sub 2}O{sub 3} nanowires exhibited a broad emission band at approximately 570 nm in the green region. In contrast, the thermally nitrided Ga{sub 2}O{sub 3} nanowires exhibited a much stronger emission band at approximately 455 nm in the blue region. Display Omitted Highlights: ► The structure and luminescence properties of thermally nitrided Ga{sub 2}O{sub 3} nanowires were examined. ► A uniform GaN shell layer was formed on the surface of the nanowires by thermal nitridation. ► The as-synthesized Ga{sub 2}O{sub 3} nanowires exhibited a broad yellow emission. ► The nitrided Ga{sub 2}O{sub 3} nanowires exhibited a much stronger blue emission band due to the GaN shell layer. -- Abstract: The structure and luminescence properties of thermally nitrided Ga{sub 2}O{sub 3} nanowires were examined. Transmission electron microscopy and X-ray diffraction confirmed the formation of a uniform GaN shell layer on the surface of the nanowires by thermal nitridation. The core and shell of the nitrided nanowires were monoclinic-structured single crystal Ga{sub 2}O{sub 3} and wurtzite-type hexagonal close-packed-structured single crystal GaN, respectively. The as-synthesized Ga{sub 2}O{sub 3} nanowires exhibited a broad emission band at approximately 570 nm in the yellow region. In contrast, the nitrided Ga{sub 2}O{sub 3} nanowires exhibited a much stronger emission band at approximately 455 nm in the blue region, which must originate from the newly formed GaN shell layer.

36 MATERIALS SCIENCE↗

Single crystalline multi-petal Cd nanoleaves prepared by thermal reduction of CdO

Highlights: ► Cd nanoleaves are obtained on abraded Cu substrate by thermal reduction of CdO. ► Vapour solid (VS) growth mechanism governs the formation of Cd nanoleaves (CdNLs). ► PL spectrum for CdNLs exhibits a strong ultraviolet (UV) emission band at 353 nm. ► UV band is attributed to interband radiative recombination under Xe illumination. -- Abstract: Multi-petal cadmium metal nanoleaves with 30–40 nm thickness were fabricated on abraded copper substrate by simple thermal reduction of cadmium oxide (CdO) powder at 1050 °C inside horizontal tube furnace (HTF) under nitrogen gas flow. The structural, compositional and morphological characterizations of the as-prepared cadmium nanoleaves (CdNLs) were performed by X-ray diffraction, energy dispersive X-ray spectroscopy, scanning electron microscopy, high resolution transmission electron microscopy and selected area electron diffraction. Non-catalytic vapour–solid (VS) process based growth mechanism governing the formation of CdNLs has been proposed and discussed briefly. Photoluminescence (PL) spectrum for CdNLs measured at room temperature exhibited a single prominent emission band at 353 nm which may either be ascribed to surface oxidation effects or interband radiative recombination under Xe light illumination.

36 MATERIALS SCIENCE↗

Synthesis and characterization of hydroxyapatite nanofiber by chemical precipitation method using surfactants

Highlights: ► We succeeded in synthesizing hydroxyapatite nano fibers by a chemical method. ► The reaction temperature is only 90 °C. ► The synthetic hydroxyapatite nano fiber is single crystal. - Abstract: We report a novel chemical precipitation route for the synthesis of hydroxyapatite (Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2}, HA) fibers using surfactants as templates. Fourier transform infrared spectroscopy (FTIR) and powder X-ray diffraction (PXRD) reveal the characteristic peaks of HA. Transmission electron microscope (TEM) and high-resolution TEM revealed the nano structure, crystallinity and morphology of the HA fibers. The morphology of the HA fibers after calcinations were characterized by scanning electron microscope (SEM). Br{sup −} ions were quickly replaced by the excess PO{sub 4}{sup 3−} ions in the solution after the addition of cetyltrime-thylammonium bromide (CTAB). Meanwhile, CTAB formed a rod-like micelles. Precursors reacted with PO{sub 4}{sup 3−} at the surface of CTAB micelles and finally formed the nanofiber structure.

36 MATERIALS SCIENCE↗

Spectroscopic analysis on the basis of Judd–Ofelt theory along [0 0 1] of Er:YVO{sub 4} grown by optical floating zone technique

Highlights: ► Synthesis and solid state reaction for Er:YVO{sub 4} is addressed. ► Single crystal growth by OFZ technique along c [0 0 1] is discussed. ► Differences in crystal morphology along a and c axes are experimentally observed. ► This is explained on the basis of difference in attachment energy. ► Spectroscopic investigations along [0 0 1] are carried out. - Abstract: 1.0 at.% erbium-doped YVO{sub 4} crystals have been grown along [0 0 1] by optical floating zone technique after optimizing the synthesis process. The circular cross-section of the grown crystals is explained on the basis of attachment energy. Using Judd–Ofelt (JO) theory the absorption and emission lines observed in absorption and photoluminescence data along [0 0 1] are characterized. JO intensity parameters as calculated are: Ω{sub 2} = 14.4389 × 10{sup −20} cm{sup 2}, Ω{sub 4} = 2.3320 × 10{sup −20} cm{sup 2} and Ω{sub 6} = 1.7794 × 10{sup −20} cm{sup 2}. For {sup 4}I{sub 13/2} → {sup 4}I{sub 15/2} transition the calculated radiative lifetime and emission cross-section are: 2.59 × 10{sup −20} cm{sup 2} and 2.45 ms, respectively.

36 MATERIALS SCIENCE↗

Controlled synthesis and thermal stability of hydroxyapatite hierarchical microstructures

Highlights: ► Hydroxyapatite hierarchical microstructures have been synthesized by a facile method. ► The morphology and size of the building units of 3D structures can be controlled. ► The hydroxyapatite with 3D structure is morphologically and structurally stable up to 800 °C. - Abstract: Hydroxyapatite (HAp) hierarchical microstructures with novel 3D morphology were prepared through a template- and surfactant-free hydrothermal homogeneous precipitation method. Field emission scanning electron microscopy (FESEM), high-resolution transmission electron microscopy (HRTEM), and X-ray diffraction (XRD) were used to characterize the morphology and composition of the synthesized products. Interestingly, the obtained HAp with 3D structure is composed of one-dimensional (1D) nanorods or two-dimensional (2D) nanoribbons, and the length and morphology of these building blocks can be controlled through controlling the pH of the reaction. The building blocks are single crystalline and have different preferential orientation growth under different pH conditions. At low pH values, octacalcium phosphate (OCP) phase formed first and then transformed into HAp phase due to the increased pH value caused by the decomposition of urea. The investigation on the thermal stability reveals that the prepared HAp hierarchical microstructures are morphologically and structurally stable up to 800 °C.

36 MATERIALS SCIENCE↗

NiO nanowall array prepared by a hydrothermal synthesis method and its enhanced electrochemical performance for lithium ion batteries

Graphical abstract: Self-supported NiO nanowall array is fabricated by a facile hydrothermal synthesis method and exhibits noticeable Li ion battery performance with good cycle life and high capacity. Highlights: ► NiO nanowall array is prepared by a hydrothermal synthesis method. ► NiO nanowall array with high capacity as anode material for Li ion battery. ► Nanowall array structure is favorable for fast ion/electron transfer. - Abstract: Free-standing quasi-single-crystalline NiO nanowall array is successfully fabricated via a simple hydrothermal synthesis method. The as-prepared NiO film exhibits a highly porous nanowall structure composed of many interconnected nanoflakes with thicknesses of ∼20 nm. The NiO nanowalls arrange vertically to the substrate resulting in the formation of extended porous net-like structure with pores of 30–300 nm. As anode material for lithium ion batteries, the quasi-single-crystalline NiO nanowall array exhibits pretty good electrochemical performances with high capacity, weaker polarization, higher coulombic efficiency and better cycling performance as compared to the dense polycrystalline NiO film. The quasi-single-crystalline NiO nanowall array presents an initial coulombic efficiency of 76% and good cycling life with a capacity of 564 mAh g{sup −1} at 0.5 A g{sup −1} after 50 cycles, higher than that of the dense polycrystalline NiO film (358 mAh g{sup −1}). The enhanced performance is due to the unique nanowall array structure providing faster ion/electron transport and better morphological stability.

36 MATERIALS SCIENCE↗

Controlled synthesis of different morphologies of TiB{sub 2} microcrystals by aluminum melt reaction method

Highlights: ► TiB{sub 2} microcrystals with different morphologies were synthesized. ► The growth of TiB{sub 2} is controlled by two-dimensional nucleation in Al melt. ► The growth of the hierarchical TiB{sub 2} microcrystals is controlled by two steps. - Abstract: TiB{sub 2} microcrystals with different morphologies, including hexagonal plate-like, tower-like and dendritic, were fabricated by aluminum melt reaction method in this study. The growth mechanisms of these microcrystals are also discussed based on the fundamental crystal growth theories. It is found that the growth of TiB{sub 2} is controlled by two-dimensional nucleation in aluminum melt. If the atomic concentration, reaction rate and atomic diffusion rate in the melt are high, TiB{sub 2} microcrystals exhibit hierarchical tower-like and dendritic morphologies. Otherwise, the single crystal of hexagonal plate-like morphology is obtained. The growth of the hierarchical TiB{sub 2} microcrystals is controlled by two steps, intermittent two-dimensional nucleation and continuous lateral spreading of layers on the growth faces.

36 MATERIALS SCIENCE↗

Crystal structure of HgGa{sub 2}Se{sub 4} under compression

Highlights: ► Single crystals of HgGa{sub 2}Se{sub 4} with defect-chalcopyrite structure were synthesized. ► HgGa{sub 2}Se{sub 4} exhibits a phase transition to a disordered rock salt structure at 17 GPa. ► HgGa{sub 2}Se{sub 4} undergoes a phase transition below 2.1 GPa to a disordered zinc blende. - Abstract: We report on high-pressure x-ray diffraction measurements up to 17.2 GPa in mercury digallium selenide (HgGa{sub 2}Se{sub 4}). The equation of state and the axial compressibilities for the low-pressure tetragonal phase have been determined and compared to related compounds. HgGa{sub 2}Se{sub 4} exhibits a phase transition on upstroke toward a disordered rock-salt structure beyond 17 GPa, while on downstroke it undergoes a phase transition below 2.1 GPa to a phase that could be assigned to a metastable zinc-blende structure with a total cation-vacancy disorder. Thermal annealing at low- and high-pressure shows that kinetics plays an important role on pressure-driven transitions.

36 MATERIALS SCIENCE↗

Crystal structure and elementary electronic properties of Bi-stabilized α-In{sub 2}Se{sub 3}

Highlights: • The introduction of Bi stabilizes α-In{sub 2}Se{sub 3} and facilitates the crystal growth. • Optical measurements show an indirect band gap. • Transport measurements show semiconducting temperature dependence. - Abstract: The introduction of Bi as a substitution for In at ∼12% in In{sub 2}Se{sub 3} stabilizes the α-polymorph and facilitates the crystal growth by the modified Bridgeman method. The crystal structure (R−3m, Z = 3, a = 3.9978(8) Å, c = 28.276(6) Å) and composition, (In{sub 0.88}Bi{sub 0.12}){sub 2}Se{sub 3}, of the crystals were determined by single crystal X-ray diffraction. The structure, of the tetradymite type, displays positional disorder within the middle Se layer. Optical measurements indicate that (In{sub 0.88}Bi{sub 0.12}){sub 2}Se{sub 3} has an indirect band gap of about 1.19 eV, shown by electronic structure calculations to be from valence band states near the Γ point to conduction band states at the L point. Resistivity and Hall effect measurements on Sn-doped crystals of composition (In{sub 0.88}Bi{sub 0.115}Sn{sub 0.005}){sub 2}Se{sub 3} show it to have a relatively high semiconducting resistivity, about 6 × 10{sup 4} Ω cm at 300 K, with an n-type carrier concentration varying from 10{sup 12}/cm{sup 3} at 300 K to 10{sup 15}/cm{sup 3} at 400 K.

36 MATERIALS SCIENCE↗

Single-crystalline CuGeO{sub 3} nanorods: Synthesis, characterization and properties

Graphical abstract: - Highlights: • Single crystalline CuGeO{sub 3} nanorods were prepared via a hydrothermal route. • The material exhibits greatly enhanced activity in photocatalytic degradation of dyes. • The magnetic susceptibility measurements indicate spin-Peierls transition properties. • CuGeO{sub 3} nanorods may be of potential application in future integrated optical devices. - Abstract: Single crystalline CuGeO{sub 3} nanorods with a diameter of 20–35 nm and a length up to 1 μm have been prepared via a facile hydrothermal route with the assistance of ethylenediamine. Some influencing factors such as the reaction time, reaction temperature, the volume of ethylenediamine were revealed to play crucial roles in the formation of the CuGeO{sub 3} nanorods. A possible growth mechanism was proposed based on the experimental results. Significantly, this is the first time that CuGeO{sub 3} was used as a photocatalyst for organic pollutant degradation under UV light irradiation. The reaction constant (k) of CuGeO{sub 3} nanorods was five times that of the sample prepared by solid-state reaction under UV light irradiation. Additionally, the optical and magnetic properties of CuGeO{sub 3} nanorods were systematically studied.

36 MATERIALS SCIENCE↗

WO{sub 3} nanoplates, hierarchical flower-like assemblies and their photocatalytic properties

Graphical abstract: WO{sub 3} nanoplates, hierarchical flower-like assemblies and their visible light-driven photocatalytic properties for degradation of rhodamine B. - Highlights: • Preparation of monoclinic WO{sub 3} by a hydrothermal reaction of PbWO{sub 4} in the presence of HNO{sub 3}. • Single-crystalline WO{sub 3} nanoplates were formed when 4 M HNO{sub 3} solution was used. • WO{sub 3} flowers were assembled by nanoplates when 15 M HNO{sub 3} solution was used. • The products showed excellent visible light-driven photodegradation of rhodamine B. - Abstract: Monoclinic WO{sub 3} was prepared by a hydrothermal reaction of PbWO{sub 4} in the presence of HNO{sub 3}. WO{sub 3} rectangular nanoplates with a side length of 50–150 nm and a thickness of about 25 nm were obtained at 4 M HNO{sub 3} solution. And the single crystal nature was confirmed by the selected area electron diffraction. Whereas WO{sub 3} hierarchical flower-like assemblies with 3–5 μm in diameter were self-organized by nanoplates in the presence of 15 M HNO{sub 3} solution. Compared with commercial WO{sub 3} particles, our products showed an enhancement of photocatalytic properties for the degradation of rhodamine B under visible light irradiation.

36 MATERIALS SCIENCE↗