Synthesis of Dy2O3 nanoparticles via hydroxide precipitation： effect of calcination temperature

This work described the preparation of dysprosium oxide, Dy2O3, nanoparticles using the homogeneous precipitation method. Dy3+ ions were precipitated using NaOH solution. The obtained product was filtered, dried, and then calcined for 1 h at the temperature range of 300–700 °C in static air. The calcination temperature of the Dy-precursor was chosen based on its decomposition as indicated by the TGA analysis. The crystalline structure and surface morphology of the calcined solids were studied by X-ray diffraction(XRD), field emission scanning electron microscopy(FE-SEM), transmission electron microscopy(TEM) and X-ray photoelectron spectroscopy(XPS). The obtained results revealed that Dy2O3 with crystallites size of 11–21 nm was formed at 500 °C. Such value increased to 25–37 nm for the sample calcined at 700 °C.     

Phase Transformation and Microstructure of Zn2Ti3O8 Nanocrystallite Powders Prepared Using the Hydrothermal Process

This paper examines the phase transformation and microstructure of Zn₂Ti₃O₈ nanocrystallite powders prepared using the hydrothermal process that includes TiCl₄ and Zn(NO₃)₂·6H₂O as the initial materials. Differential thermal analysis, X-ray diffraction, transmission electron microscopy (TEM), selected area electron diffraction, nanobeam electron diffraction, and high resolution TEM were utilized to characterize the transition behavior of zinc titanate precursor powders after calcination. Nanocrystalline Zn₂Ti₃O₈ powders with a size range of about 5.0 to 8.0 nm were obtained when the precursor powders were calcined at 773 K (500 °C) for 1 hour. When the zinc titanate precursor powders were calcined at 1073 K (800 °C) for 1 hour, the cubic crystal of Zn₂Ti₃O₈ with a _o = 0.8399 ± 0.0003 nm still remained the predominant crystalline phase and the crystallite size increased to 20.0 nm. In addition, ZnTiO₃ phase first appeared because of the 13.8 pct of Zn₂Ti₃O₈ decomposition when the zinc titanate precursor powders were calcined at 1073 K (800 °C) for 1 hour. When the zinc titanate precursor powders were calcined at 1073 K (800 °C) for 9 hours, the Zn₂Ti₃O₈ crystallites grew continuously to 80.0 nm and enhanced the crystallinity. When the precursor powders were calcined at 1273 K (1000 °C) for 1 hour, Zn₂TiO₄ crystallites with a _o = 0.8461 ± 0.0002 nm were the predominant crystalline phase.     

Luminescent characterization of rare earth Dy3+ ion doped TiO2 prepared by simple chemical co-precipitation method

Pure and rare-earth ion (Dy³⁺) doped TiO₂ nanomaterials were prepared through a chemical co-precipitation method. The chemical composition, microstructure and optical properties were characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), UV-visible spectroscopy and photoluminescence (PL). XPS analysis reveals that Dy³⁺ ions are preferentially occupied in the TiO₂ crystallite lattices. Both the XRD and TEM analyses confirm that both the pure and Dy doped TiO₂ are in pure anatase phase and in nano size range, respectively. Also it is found that the maximum solubility limit for Dy³⁺ ions is found to be 0.4% in TiO₂ matrix, above which it occupies interstitials and/or crystallite surface of TiO₂ nanocrystals. From the UV-Vis spectroscopy studies it is found that Dy doping induces blue shift in TiO₂. From the PL analysis it is found that doping Dy³⁺ improves the luminescence behavior in comparison with the pure TiO₂ nanoparticles. Overall, doping very low concentrations of Dy³⁺ greatly alters the structural morphology and directly increases the luminescence behavior of TiO₂ suitable for advanced optoelectronic applications.     

Oxidation of Ti3SiC2 composites in air

The oxidation of Ti₃SiC₂ composites (75 at. pct Ti₃SiC₂ and 25 at. pct TiC _x ), prepared via self-propagating high-temperature synthesis (SHS) and subsequent shock consolidation, has been studied in the range of 1073 to 1573 K in this research. The oxidation kinetics are parabolic with an activation energy of approximately 240±20 kJ/mol. As shown by transmission electron microscopy (TEM) during the very early stages of oxidation, the oxide layer formed contains amorphous SiO₂ and crystalline rutile (TiO₂). As oxidation proceeds, a two-layered oxide scale is observed with the outer oxide layer consisting of columnar TiO₂ with trace amounts of SiO₂ and the inner oxide layer being comprised of a mixture of amorphous SiO₂ and fine crystalline TiO₂. The grain size of the outermost oxide (TiO₂) increases with increasing oxidation temperature. The oxidation resistance of the Ti₃SiC₂ composites prepared by SHS and subsequent shock consolidation is similar to the oxidation of Ti₃SiC₂ prepared by other means with comparable parabolic constants.     

Luminescence properties of dysprosium doped YVO4 phosphor

Trivalent dysprosium(Dy~(3+)) activated nanocrystalline yttrium vanadate(YVO_4) phosphor was synthesized via co-precipitation method. The prepared samples were characterized by X-ray diffraction(XRD),Fourier transform infrared spectroscopy(FTIR), scanning electron microscopy(SEM), optical absorption and photo luminescence(PL) techniques. The XRD patterns reveal the tetragonal crystalline phase. SEM images reveal that Dy doped YVO_4 nanocrystals are agglomerated. EDAX confirms the formation of YVO_4:Dy. FTIR spectrum shows two strong absorption bands at 459 and 761 cm~(-1). Optical absorption spectrum showed the surface defects in the as-prepared samples. The PL emission spectrum shows two characteristic emission bands at 485 and 575 nm. The strong yellow emission peak at 575 nm is assigned to ~4 F_(9/2)→~6 H_(13/2) hyper sensitive transition of Dy~(3+) ions, Study of CIE chromaticity diagram indicates the suitability of the phosphor for the development of yellow-green LEDs.     

Synthesis of nanostructured spherical aluminum oxide powders by plasma engineering

Irregularly shaped aluminum oxide particles were plasma atomized resulting in narrow size range distribution of spherical nanostructured powders. Cooling rates, on the order of 10⁶ to 10⁸ K/s, were obtained from the different quenching medias, viz. air, water, and liquid nitrogen. Plasma-engineered powder particles developed nanosize crystallites, while solidification provided insight into the morphological feasibility in refinement of grain size. X-ray diffraction (XRD) methods have been used to quantify the crystallite size obtained with different quenching media. Raman peak shift validated the X-ray analysis in anticipating the grain refinement with increasing cooling rates. Salient structural morphology characteristics and a detailed understanding of spheroidized plasma-sprayed alumina powders were analyzed through scanning electron microscopy (SEM) studies. Formation of nanograins, novel metastable phases, and amorphous structure were endorsed by transmission electron microscopy (TEM) investigations.     

The effect of reaction condition on composition and properties of ultrafine amorphous powders in (Fe,Co, Ni)-b systems prepared by chemical reduction

Amorphous ultrafine powders in (Fe, Co, Ni)-B binary systems were prepared in different reduction conditions of metal ions in an aqueous solution by use of KBH₄, with the aim of clarifying the effect of reaction conditions on the composition, thermal stability, and magnetic properties of the resultant amorphous powders. As the mol ratio of KBH₄ to metal ions decreases, the structure of the ultrafine powders changes from amorphous to crystalline phase. The morphology of these powders is in a nearly spherical shape with a particle size of about 20 nm for the amorphous phase and changes to the chain-like or net-like shape for the crystalline phase. The B content in the Fe-B amorphous powder decreases with a decrease of the ratio of KBH₄ to metal ions, and the powder size decreases with an increase of the reduction temperature.     

Amorphization of Al50(Fe2B)30Nb20 Mixture by Mechanical Alloying

An amorphous Al₅₀(Fe₂B)₃₀Nb₂₀ powder mixture was prepared by mechanical alloying in a high-energy planetary ball-mill under argon atmosphere. Morphologic, microstructural, and structural changes during the milling process were followed by scanning electron microscopy and X-ray diffraction. Rietveld analysis of X-ray diffraction patterns was used to follow the solid-state amorphization transformation during the milling process of the prepared powder. The reaction between elemental Al, Fe₂B, and Nb powders leads to the formation of the Al(Fe,B) and Al(Fe,Nb,B) solid solutions after 4 and 6 hours of milling, respectively. An amorphous structure is achieved after 20 of milling. These amorphous powders are crystallized on further milling time (36 hours). The observation by scanning electron microscope shows a phenomenon of fracturing followed by compaction of the powder particles.     

Stabilization of the fluorite phase in the ZrO<Subscript>2</Subscript>–Y<Subscript>2</Subscript>O<Subscript>3</Subscript> system

The calculated and experimental vertical ZrO₂–Y₂O₃ sections of the Zr–Y–O system are compared to find the region of a stable fluorite structure of yttrium-stabilized zirconia (YSZ). X-ray diffraction (XRD) and Raman scattering are used to study the crystal and local structures of mixed oxide 0.82ZrO₂ · 0.18Y₂O₃ (18YSZ) powders prepared by isothermal annealing of a precursor precipitated from a salt solution. The formation of a fluorite-type fcc structure (space group \(Fm\overline 3 m\)) in the powders is detected by XRD. Raman scattering study of the local structure of the cubic 18YSZ powders revealed traces of the tetragonal phase in them.     

Phase composition of the vanadium-containing titanium slags forming upon the reduction smelting of the titanomagnetite concentrate from the Kuranakhsk deposit

The phase composition of the vanadium-containing titanium slags that form upon the reduction smelting of the titanomagnetite concentrate from the Kuranakhsk deposit with an added CaCO₃ flux is studied by optical microscopy, X-ray diffraction, and scanning electron microscopy. The laws of formation of the phase composition and the interphase distribution of vanadium and other elements are revealed as a function the CaO and FeO contents in the slags. It is shown that, at low CaO contents (up to 5%), the phase composition of the slags containing 15–30% FeO is mainly represented by spinelides (Al-V-Cr and Al-Ti-V spinels and (Fe,Mg)₂TiO₄ ulvospinel), anosovite, and glass. When the CaO content in slag increases, titanium is fixed into perovskite. At 17–20% CaO and ≤8.3% FeO in slag, a new crystalline phase, i.e., Ca-Al-V titanate of a complex composition, forms along with perovskite, the Al-V-Cr spinel, anosovite, and glass. Vanadium in the slags is mainly distributed between anosovite, the spinelides, and the Ca-Al-V titanate, and vanadium is absent in the glassy phase.     

Effects of Dysprosium Oxide Doping on Microstructure and Properties of Barium Titanate Ceramic

With the development of mixed integrated cir-cuits , mini mization of high voltage ceramic capacitorcomponents usedin high voltage outletsis required .Inthe past ,the breakdown voltage was raised mainly byincreasingthethickness of capacitors .Butthe most …     

Laser Absorbency of Samarium Borate Prepared by Solid-State Reaction

Submicron SmBO₃ powders were prepared by solid-state reaction method using H₃BO₃ and Sm₂O₃ powders as starting materials. The phase evolution, morphologies and laser absorbency of the synthesized powders were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR) and reflectivity analyzer. The results showed that the powders calcined at 800 °C consisted of a little amount of intermediate phase of Sm(BO₂)₃ besides the main crystalline phase of SmBO₃. However, at 900 °C, the intermediate phase disappeared and the single, pure SmBO₃ phase was obtained. The prepared powders were aggregated and uniform with irregular morphologies and an average original particle size of about 500 nm. The FTIR showed that an apparent absorbent peak appeared at the wavelength of 10.6 μm laser. Moreover, the reflectivity of the powders apparently decreased at the wavelength of 1.064 μm laser. The synthesized SmBO₃ powders might may be a kind of promising absorbent of laser camouflage materials.     

Synthesis and luminescence properties of SrAleO4：Eue＋,Dy3＋ hollow microspheres via a solvothermal co-precipitation method

SrAl2O4:Eu2+,Dy3+ hollow microspheres were successfully prepared through a facile and mild solvothermal co-precipitation combining with a postcalcining process.The structure and particle morphology were investigated by X-ray diffraction(XRD),scanning and transmission electron microscopy(SEM and TEM)pictures,respectively.The mechanism for the formation of spherical SrAl2O4:Eu2+,Dy3+ phosphor was preliminary presented.After being irradiated with ultraviolet(UV)light,the spherical phosphor emitted long-lasting green phosphorescence.Both the photoluminescence(PL)spectra and luminance decay,compared with that of commercial bulky powders,revealed that the phosphors had efficient luminescent and long lasting properties.It was considered that the SrAl2O4:Eu2+,Dy3+ hollow microspheres had promising long-lasting phosphorescence with potential scale-dependent applications in photonic devices.     

The Effect of the Amorphous and Crystalline States on Preferential Corrosion of Hf from a Cu75Hf20Dy05 Alloy

Amorphous solid-solution Cu₇₅Hf₂₀Dy₀₅, which undergoes devitrification without changing composition either locally or globally, was used to examine the effects of structural ordering on corrosion properties in the absence of any accompanying chemical partitioning. Melt spun amorphous Cu₇₅Hf₂₀Dy₀₅ undergoes single-phase devitrification to a Cu₅₁Hf₁₄ phase. The difference in corrosion behavior between these two structures was explored in hydrofluoric acid solutions where preferential dissolution of hafnium occurred. Preferential Hf dissolution occurred more readily in the amorphous alloy compared with its crystalline counterpart. Remaining copper reorganized to form a face-centered cubic (fcc) nanostructure in both conditions, but this process occurred quickly in the amorphous state and more slowly in the crystalline variant. A uniform, nanoporous Cu sponge structure, with a pore diameter of approximately 10?nm, formed after dissolution in the amorphous state. A less uniform, nanoporous structure developed more slowly when occurring from the crystalline state. These differences were traced to the effects of ordering on both dissolution and surface diffusion.     

低发射率SiO2/Al2 O3纳米复合粉体的制备和红外隐身性能

采用溶胶-凝胶法制备非晶态和结晶态两种相结构的SiO₂/Al₂O₃纳米复合粉体,通过X射线衍射、透射电子显微镜等手段对纳米复合粉体结构和形貌进行表征,并利用傅里叶变换红外光谱仪研究纳米复合粉体的红外隐身性能.结果表明:两种相结构的SiO₂/Al₂O₃纳米复合粉体均呈不规则颗粒状,其中结晶态SiO₂/Al₂O₃纳米复合粉体的平均晶粒尺寸约为18 nm;结晶态SiO₂/Al₂O₃纳米复合粉体在2.5~25μm波长范围内的红外发射率均低于非晶态复合粉体,3~5μm内发射率平均值为45.65%,8~14μm内发射率平均值为46.19%,是一种低发射率的红外隐身复合纳米材料.      

Joint solubility of samarium and dysprosium in solid magnesium

The phase compositions of solid Mg–Sm–Dy alloys corresponding to the magnesium-corner region of the phase diagram are studied by optical and scanning electron microscopy, electrical resistivity measurements, and electron microprobe analysis. The obtained results allowed us to determine the joint solubility of samarium and dysprosium in solid magnesium at 500, 400, and 300°C; it decreases with decreasing temperature. The magnesium solid solution is found to be in equilibrium only with the Mg₄₁Sm₅ and Mg₂₄Dy₅ compounds, which are in equilibrium with the magnesium solid solution in the binary Mg–Sm and Mg–Dy systems.     

Morphological and calorimetric studies on the

Amorphous Al₅₀Zr₅₀ alloy powders have been prepared by rod-milling technique using mechanical alloying (MA) method. The amorphization and crystallization processes of the alloyed powders were followed by optical microscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), differential thermal analysis (DTA), and differential scanning calorimetry (DSC). The results have shown that the formation of amorphous Al₅₀Zr₅₀ alloy powders occurs through three stages, agglomeration, disintegration, and homogenization. At the disintegration stage, the alloyed powders contain many fine layers of Al and Zr. An amorphous phase has been formed at about 880 K as a result of heating these layered particles in a thermal analyzer. The crystalline-to-amorphous transformation at this stage of milling is attributed to a thermally assisted solid-state amorphizing reaction. The present study corroborates the similarity of the amorphization process through the MA with the solid-state interdiffusion reaction in multilayered thin films. The amorphization temperature, T_a, and the activation energy of amorphization, E_a, are 675 and 156 kJ/mol, respectively. In addition, the enthalpy change of amorphization, ΔH_a, was evaluated to be -3.5 kJ/mol. On the other hand, the crystallization temperature, T_x, and enthalpy change of crystallization, ΔH_x, were 1000 K and −68 kJ/mol, respectively.     

Structural study of electrodeposited aluminum-manganese alloys

Aluminum-manganese alloys with compositions ranging between 0 and 27 wt pct Mn were electrodeposited at 150°C onto copper substrates from a chloroaluminate molten salt electrolyte with a controlled addition of MnCl₂. The specimens were studied by scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive spectroscopy (EDS), and X-ray diffraction. The addition of small amounts of Mn results in the formation of a supersaturated fcc solid solution of Mn in Al. At the higher Mn content, an amorphous phase is established. The highly faceted crystalline surface of pure Al and Al−Mn solid solution becomes smooth and nearly specular when the amorphous phase is present. The amorphous phase appears in the form of rounded grains and has a lower limit of Mn concentration close to the Al₆Mn composition. There is a concentration discontinuity between the above limit and the higher Mn concentration limit of the fcc phase (about 9 wt pct). Appearance of the amorphous phase in the alloy results in a decrease in the Mn concentration in solid solution to about 2 wt pct. Crystallization of the amorphous phase starts at the fcc-amorphous phase interface at 230°C. As a result of treatment at 230 °C to 340 °C, the amorphous phase completely transforms into Al₆Mn, while the fcc phase is unaffected. Prior to crystallization, the amorphous phase shows a modification that could be interpreted as the formation of a fine-grained icosahedral phase. The formation and distribution of phases by electrodeposition and rapid solidification are discussed.     

Relationship between controllable preparation and microstructure of NdFeB sintered magnets

The double hard magnetic phase magnets with nominal compositions of Nd_30–xDy_xFe₆₉B₁(x=2, and 4) (wt.%) were prepared. The magnetic properties of the magnets were measured with a NIM-2000H hysteresigraph. The crystalline structures of the magnets were identified by X-ray diffraction (XRD). The Rietveld refinement was carried out using the FULLPROF software. The scanning electron microscopy (SEM) and transmission electron microscopy (TEM) analyses were carried out in order to investigate the microstructure of the magnets. It showed that the magnets consisted mainly of Nd₂Fe₁₄B phase, and some Nd-rich phase. Two types of matrix-phase grains in dark grey and light grey were found in the magnets with x=2 and 4. The Dy content was obviously different in the two types of grains, which proved that the double hard magnetic phases (Dy-rich and Dy-lean phases) coexisted in the magnet. It revealed that the Nd-rich phases in junction regions had fcc structure, with the unit cell parameter of about 0.52–0.56 nm. The weak superlattice spots were found in the SAD patterns of the junction Nd-rich phases with large scale. The double hard magnetic phase structure seemed to improve the magnetic properties of NdFeB magnets with high coercivity, while decrease the consumption of Dy element, compared with the single alloy magnet.     

Diary

Abstract

The addition of amorphous Fe–Si–B particles to Fe powder increases the shrinkage of sintered components resulting in higher densification rates. Consequently, several research groups worldwide have studied the properties of such systems in an attempt to produce superior structural alloys. In the present work, Fe₇₅Si₁₀B₁₅ ribbons obtained by melt spinning were milled in a high energy Spex mill for times varying from 2 to 32 h. The resulting powders were characterised by differential thermal analysis and X-ray diffraction. The results showed that the amorphous characteristics of the ribbons persisted after the milling process. Next, samples consisting of a mixture of Fe powder and 4 wt-% milled amorphous phase were uniaxially pressed and sintered following a series of thermal cycles. High temperature microstructures were obtained for compacts subjected to rapid cooling from the sintering temperature. The results of scanning electron microscopy and energy dispersive spectroscopy revealed substantial precipitation of fine Fe₂B particles before α → γ allotropic transformation. In addition, an oxide phase was observed in the interface between Fe and the additive particles. Preliminary analysis suggested that the oxide particles can be easily reduced by adding small amounts of carbon to the system. PM/0765