Effect of trace HA on microstructure,mechanical properties and corrosion behavior of Mg-2Zn-0.5Sr alloy

Effect of the addition of trace HA particles into Mg-2Zn-0.5Sr on microstructure, mechanical properties, and bio-corrosion behavior was investigated in comparison with pure Mg. Microstructures of the Mg-2Zn-0.5Sr-xHA composites(x = 0, 0.1 and 0.3 wt%) were characterized by optical microscopy(OM),scanning electron microscopy(SEM) equipped with energy dispersion spectroscopy(EDS) and X-ray diffraction(XRD). Results of tensile tests at room temperature show that yield strength(YS) of Mg-2Zn-0.5Sr/HA composites increases significantly, but the ultimate tensile strength(UTS) and elongation decrease with the addition of HA particles from 0 up to 0.3 wt%. Bio-corrosion behavior was investigated by immersion tests and electrochemical tests. Electrochemical tests show that corrosion potential(Ecorr)of Mg-2Zn-0.5Sr/HA composites significantly shifts toward nobler direction from-1724 to-1660 m VSCE and the corrosion current density decreases from 479.8 to 280.8 μA cm~(-2) with the addition of HA particles. Immersion tests show that average corrosion rate of Mg-2Zn-0.5Sr/HA composites decreases from11.7 to 9.1 mm/year with the addition of HA particles from 0 wt% up to 0.3 wt%. Both microstructure and mechanical properties can be attributed to grain refinement and mechanical bonding of HA particles with second phases and α-Mg matrix. Bio-corrosion behavior can be attributed to grain refinement and the formation of a stable and dense CaHPO_4 protective film due to the adsorption of Ca~(2+)on HA particles. Our analysis shows that the Mg-2Zn-0.5Sr/0.3HA with good strength and corrosion resistance can be a good material candidate for biomedical applications.     

Atomic scale study of the dehydration/structural transformation in micro and nanostructured brucite (Mg(OH)2) particles: Influence of the hydrothermal synthesis conditions

Micro and nanostructured brucite (Mg(OH₂)) particles synthesized by hydrothermal method from solutions with high content of hydrazine (0.14 M) and nitrate (0.24 g) were compared with samples obtained from low hydrazine content (0.0002 M) and nitrate (0.12 g). The samples were heated at 180 °C for 4 h, 6 h and 12 h. XRD, TEM-HRTEM, SAED and image analysis techniques were used for the morphological and structural characterization. The effect of electron beam irradiation on the brucite dehydration was observed in atomic resolution images at 300 kV. Hexagonal crystals show differences in crystallinity, strains and kinetic of reaction. High hydrazine/nitrate samples have slightly larger crystals with better crystallinity, showing a strong preferential orientation. Rietveld refinements show how unit cell parameters are bigger in samples obtained with higher hydrazine/nitrate content, confirming also the preferential orientation along the 0 0 0 1 plane. Differences in the dehydration process show the rapid formation of a porous surface, the amorphised cortex or the presence of highly oriented strains in samples prepared from higher hydrazine/nitrate content. Conversely, crystals slightly smaller with randomly scattered defect surfaces showing the Mg(OH)₂/MgO interphase in samples prepared with low hydrazine/nitrate content. Significant differences in the kinetic of reaction indicate how the dehydration process is faster in samples prepared with high hydrazine/nitrate content.     

A novel red phosphor Na2Ca4Mg2Si4O15:Eu3+ for plasma display panels

A novel red emitting phosphor, Eu³⁺-doped Na₂Ca₄Mg₂Si₄O₁₅, was prepared by the solid-state reaction. X-ray powder diffraction (XRD) analysis confirmed the formation of Na₂Ca₄Mg₂Si₄O₁₅:Eu³⁺. Field-emission scanning electron-microscopy (FE-SEM) observation indicated a narrow size-distribution of about 300 nm for the particles with spherical shape. Upon excitation with vacuum ultraviolet (VUV) and near UV light, the phosphor showed strong red-emission lines at around 611 and 617 nm, respectively, corresponding to the forced electric dipole ⁵D₀ → ⁷F₂ transition of Eu³⁺, and the highest PL intensity at 617 nm was found at a content of about 8 mol% Eu³⁺. The optical properties study suggests that it is a potential candidate for plasma display panels (PDPs) application.     

Spectroscopic properties of Tm3+/Al3+ co-doped sol–gel silica glass

Tm³⁺/Al³⁺ co-doped silica glass was prepared by sol–gel method combined with high temperature sintering. Glasses with compositions of xTm₂O₃–15xAl₂O₃–(100 − 16x) SiO₂ (in mol%, x = 0.1, 0.3, 0.5, 0.8 and 1.0) were prepared. The high thulium doped silica glass was realized. Their spectroscopic parameters were calculated and analyzed by Judd–Ofelt theory. Large absorption cross section (4.65 × 10⁻²¹ cm² at 1668 nm) and stimulated emission cross section (6.00 × 10⁻²¹ cm² at 1812 nm), as well as low hydroxyl content (0.180 cm⁻¹), long fluorescence lifetime (834 μs at 1800 nm), large σ_em × τ_rad (30.05 × 10⁻²¹ cm² ms) and large relative intensity ratio of the 1.8 μm (³F₄ → ³H₆) to 1.46 (³H₄ → ³F₄) emissions (90.33) are achieved in this Tm³⁺/Al³⁺ co-doped silica glasses. According to emission characteristics, the optimum thulium doping concentration is around 0.8 mol%. The cross relaxation (CR) between ground and excited states of Tm³⁺ ions was used to explain the optimum thulium doping concentration. These results suggest that the sol–gel method is an effective way to prepare Tm³⁺ doped silica glass with high Tm³⁺ doping and prospective spectroscopic properties.     

Rapid hydrothermal synthesis of SrMo1−xWxO4 powders: Structure and luminescence characterization

Strontium molybdate, strontium tungstate particles and their solid solutions (SrMo_1?xW_xO₄) with 0 ? x ? 1.0, were synthesised by means of a hydrothermal process. Crystallisation of SrMo_1?xW_xO₄ particles took place rapidly using SrSO₄ as the Sr precursor under hydrothermal conditions involving stirring (130 rpm) at 150 or 200 °C for 2 h. Structural analyses of the powders were conducted by XRD with Rietveld refinement and FT-Raman spectroscopy, and the particle shape was observed by FE-SEM. Lattice parameter measurements indicated a linear dependence of both “a₀” and “c₀” in the scheelite structured SrMo_1?xW_xO₄ with a changing W content following Vegard’s law. These analyses also provided evidence of the structural variation localised in the tetrahedral site as a result of the simultaneous incorporation of MoO₄ and WO₄ in the solid solutions formed in the compositional range of 9 ? x ? 60 mol%. The SrMo_1?xW_xO₄ particles exhibited a predominantly euhedral shuttle-shaped morphology and particle sizes varying between 0.75 and 1.5 μm. The particle growth was affected by increasing the reaction temperature and the tungsten concentration. Photoluminescence analysis (PL) revealed a marked attenuation of the blue and green emissions preferentially for the powder containing 48.5 mol% of W, which makes it potentially useful for optoelectronic applications.     

Synthesis and photoluminescence of Ca1-xTiO3:xEu3+ nanoparticles

Ca_1-xTiO₃:xEu³⁺ nanoparticles (NPs) with the size ranging from 27 nm to 135 nm were prepared by means of a chemical co-precipitation method. The structural and optical properties of the NPs were investigated, and the influence of Eu doping content and sintering temperature on the photoluminescence of the Ca_1-xTiO₃:xEu³⁺ NPs were examined. An obvious red emission band centered at 615 nm were observed under the excitation with 395 nm for the Ca_1-xTiO₃:xEu³⁺ NPs. X-ray photoelectron spectroscopy analyses suggest that Eu³⁺ is incorporated into not only the Ca-site, but also Ti-site of CaTiO₃ crystal lattice. Our study shows the promise of the Ca_1-xTiO₃:xEu³⁺ NPs as a red nanophosphor.     

Photoluminescence of CaAlSiN3:Eu2+-based fine red-emitting phosphors synthesized by carbothermal reduction and nitridation method

In this research, we have presented the synthesis and characterization of the various Ca_1−xEu_xAl_0.76Si_1.18N₃ (x = 0.01 ∼ 0.1) red-emitting phosphors, which were successfully prepared by carbothermal reduction and nitridation (CTRN) method without the strict needs of high pressure. Here, raw materials were CaCO₃, AlN, Si₃N₄, Eu₂O₃, and C. In particular, C was considered as efficient and robust reducing agent. The influences of reaction temperature, holding time, C content, and Eu²⁺ concentration were investigated in the crystal phase compositions and photoluminescence properties of the as-prepared phosphors. Importantly, CaAlSiN₃:Eu²⁺-based red phosphors with interesting properties were obtained with reaction temperature at 1600 °C for 4 h by atmospheric N₂–10%H₂ pressure, and the C/O ratio of 1.5:1, respectively. The emission peak positions of as-prepared phosphors were red-shifted from 607 nm to 654 nm with Eu²⁺ concentration from 1 mol% to 10 mol%. Meanwhile the highest luminescence intensity was achieved with 2 mol% of Eu²⁺ concentration, which showed high external quantum efficiency up to 71%. Combining the phosphor blend of green-emitting β-sialon:Eu²⁺, yellow-emitting Ca-α-sialon:Eu²⁺, and red-emitting Ca_0.98Eu_0.02Al_0.76Si_1.18N₃ with a blue LED (light emitting diodes), warm white LED can be generated, yielding the color rendering index (Ra) of 93 at correlated color temperature (CCT) of 3295 K. These results indicate that CaAlSiN₃:Eu²⁺-based red-emitting phosphors prepared by facile CTRN are highly promising candidates for warm white LEDs.     

Photoluminescence properties of Eu2+-activated Ca2Y2Si2O9 phosphor

Eu²⁺-activated Ca₂Y₂Si₂O₉ phosphors with different Eu²⁺ concentrations have been prepared by a solid-state reaction method at high temperature and their photoluminescence (PL) properties were investigated. Photoluminescence results show that Eu²⁺-doped Ca₂Y₂Si₂O₉ can be efficiently excited by UV–visible light from 300 to 425 nm. Ca₂Y₂Si₂O₉: Eu²⁺ exhibits broad band emission in the wavelength range of 425–700 nm, due to the 4f⁶5d¹ → 4f⁷5d⁰ transition of the Eu²⁺ ions located at two different sites ((Ca/Y)1 and (Ca/Y)2) in Ca₂Y₂Si₂O₉. The effect of the Eu²⁺ concentration in Ca₂Y₂Si₂O₉ on the PL properties was investigated in detail. The results showed that the relative PL intensity reaches a maximum at 1 mol% of Eu²⁺, and a red-shift of the emission bands from these two different sites was observed with increasing Eu²⁺ concentration. Also there exists energy transfer between these two Eu²⁺ sites. The potential applications of Ca₂Y₂Si₂O₉: Eu²⁺ have been pointed out.     

Microstructure correlated electrical conductivity of Manganese alloyed nanocrystalline cubic zirconia synthesized by mechanical alloying

Fully stabilized cubic (c) ZrO₂ phase has been synthesized by mechanical alloying (MA) the stoichiometric powder mixture of elemental Mn (5–20 mol%) and monoclinic (m) ZrO₂ at room temperature. XPS study reveals that major part of metallic Mn is ionized to Mn²⁺ oxidation state during MA. Mn-alloyed c-ZrO₂ nanoparticles with ～18 nm particle size have been synthesized within 10 h of MA. Microstructures of the compounds have been precisely evaluated by analyzing the X-ray powder diffraction patterns employing Rietveld refinement and transmission electron microscopy images. A decrease in lattice parameter from 5.11 Å to 5.09 Å is correlated with an increase in oxygen vacancy from 14% to 26% with increasing Mn concentrations. Elemental compositions in the compounds are obtained from electron probe microanalysis. The role of Mn alloying in the polymorphic phase transformation (m → c) has been established with changes in structure and microstructure parameters. Electrical conductivities of all c-ZrO₂ compounds are measured in the temperature range 350–550 °C. Grain and grain boundary contributions to total conductivity are calculated from frequency dependent real and imaginary impedance. Conductivity of Mn alloyed c-ZrO₂ increases with increasing temperature and Mn concentrations. Electrical transport mechanism in the compound is studied by impedance and modulus spectroscopy. The relaxation frequency is found to be temperature, microstructure and composition dependent.     

Fabrication of (Ca + Yb)- and (Ca + Sr)-stabilized α-SiAlON by combustion synthesis

In this paper, (Ca + Yb)- and (Ca + Sr)-stabilized α-SiAlON powders were fabricated by combustion synthesis. The influence of Ca²⁺ incorporation on the phase composition and grain morphology of combustion products was discussed. The experimental results showed that with the incorporation of Ca²⁺ well-developed rod-like (Ca + Yb) α-SiAlON crystals could be produced. It was also found that, when only Sr²⁺ was used as stabilizing cation, the reaction product was (α + β)-SiAlON composite, in which β-SiAlON was the predominant phase and the relative content of α-SiAlON was low. With the incorporation of Ca²⁺, however, both the relative content and the lattice parameters of α-SiAlON were clearly increased. These results indicated that the incorporation of Ca²⁺ could assist Sr²⁺ into the α-SiAlON lattice structure.     

Influence of temperature, [Ca2+], Ca/P ratio and ultrasonic power on the crystallinity and morphology of hydroxyapatite nanoparticles prepared with a novel ultrasonic precipitation method

Nanocrystalline hydroxyapatite was prepared by a precipitation method with the aid of ultrasonic irradiation using Ca(NO₃)₂ and NH₄H₂PO₄ as source material and carbamide (NH₂CONH₂) as precipitator. The influence of Ca/P molar ratio, precipitation temperature, concentration of Ca²⁺ ([Ca²⁺]) and ultrasonic power on the crystallinity of the nanopowder were systematically investigated by XRD analysis. The size of the as-prepared particles was analyzed using TEM and XRD methods. The results revealed that the monophase hydroxyapatite could be obtained at the following technological conditions: [Ca²⁺] = 0.01–0.1 mol/L, ultrasonic power = 300 W, Ca/P (mol) = 1.2–2.5 and T = 313–353 K. In addition, the acicular and spherical particles could be prepared at different ultrasonic powers of 300 and 200 W, respectively.     

Synthesis of mesoporous geopolymeric powder from LD slag as superior adsorbent for Zinc (II) removal

Linz-Donawitz(LD) slag Geopolymer(LDSGP), a porous aluminosillicate geopolymeric adsorbent, has been synthesized from steel plant LD slag for efficient removal of Zinc(II) ions from wastewater, thus presenting a solution for converting industrial waste to adsorbent for wastewater treatment. The colloid paste of raw LD slag and the alkaline activator (10?M NaOH?+?sodium silicate (1:1 w/w)) has been cured for 3?days at low temperature to geopolymerize the calcium oxide rich LD slag. The BET surface area of LDSGP adsorbent (30.84?m²/g) has improved considerably compared to raw LDS (4.85?m²/g) and the FESEM and HRTEM images reveal the presence of micropetal and cauliflower like structures at outer surface of the adsorbent particles. The mesoporous nature of LDSGP adsorbent can be understood by analyzing N₂ adsorption-desorption and pore size distribution plot. The PXRD pattern of LDSGP adsorbent powder confirms the presence of Ca₂SiO₄ and Ca₃SiO₅ in the geopolymeric matrix. Langmuir isotherm model correlates the batch adsorption data of Zn²⁺ ions onto LDSGP particles at 298?K, 308?K and 318?K. The maximum Zn²⁺ ions adsorption capacity of LDSGP is 86?mg/g at 318?K. The adsorption kinetic data is correlated with pseudo-second-order model indicating chemisorption of Zn²⁺ ions onto LD slag geopolymeric powder adsorbent.     

Molten-salt synthesis of tetragonal micron-sized barium titanate from a peroxo-hydroxide precursor

Barium titanate (BaTiO₃) was produced from an barium-titanate-peroxo-hydroxide precursor material in NaCl-KCl and Na₂SO₄-K₂SO₄ salt mixtures or fluxes at temperatures up to 1080 °C via the molten-salt synthesis (MSS) method. Beside the different salt mixtures several other parameters were studied to determine the effect on the particle morphology. A relatively fast heating rate and a relatively high salt to precursor ratio resulted in a highly faceted morphology. The effect of the salt flux was clearly seen in the morphology of BaTiO₃ obtained by MSS at 1080 °C. Cube-shaped particles were observed for the chloride-flux-grown BaTiO₃ while hexagonal-shaped flat particles were observed for the sulfate-flux-grown BaTiO₃. BaTiO₃ particles produced in the chloride-flux were either {1 0 1} or {0 0 1} faceted. The hexagonal surface of the sulfate-flux-grown BaTiO₃ was {1 1 1} faceted.     

The effect of Eu3+ concentration on the Y2O3 host lattice obtained from citrate precursors

This work presents a thermal decomposition study of the precursor resin prepared from the citrate precursor along with structural features and optical properties materials composed by Y₂O₃ and Eu³⁺ containing Y₂O₃ in 0.5, 3, 5 and 7 mol%. The microcrystallite sizes were estimated from the Scherrer equation. The structural and optical properties revealed that the addition of 5 mol% of Eu³⁺ to the Y₂O₃ matrix gave rise to the highest relative emission intensity which was evidenced by the luminescence intensity. The lifetime of the 0.5 mol% Eu³⁺-doped sample suggested two different symmetry sites for Eu³⁺ ions because two different lifetime values were acquired for this sample, while for phosphors doped with 3 or 5 mol% of Eu³⁺ ions only one similar lifetime was observed. When the concentration of Eu³⁺ is 0.5 and 3 mol%, the luminescence intensity is weak due to the low probability of the O^2? - Eu³⁺ charge transfer transition. On the other hand, when the concentration of the Eu³⁺ ions is 7 mol%, a quenching effect is evidenced.     

Preparation of spherical silica in emulsion systems using the co-precipitation technique

Silica powders with particles of spherical shape and a low tendency to agglomeration of primary particles have been prepared by precipitation from sodium metasilicate and hydrochloric acid via the emulsion technique. The organic phase of the emulsion system was cyclohexane while a non-ionic surfactant was applied as an emulsifier. In the course of silica precipitation three alternative ways of dispersion induction were applied: the top stirrer, homogenization and ultrasounds. The precipitation was performed at three temperatures (25 °C, 40 °C and 60 °C), using different variants of dosing schemes of the emulsion and the aqueous solutions of substrates. Homogenization of the reactive system yielded silica of spherical particles of the lowest mean particle diameter and the most uniform character. The only appropriate mode of dosing the reagents to the emulsion was the introduction of alkaline emulsion to acidic emulsion. A decreased tendency for silica particles agglomeration could be achieved by increasing the volume of the organic phase in the emulsions prepared. The optimum temperature for the precipitation reaction was 25 °C. The procedure permitted obtaining in SiO₂ particles of the optimum diameter (<1 μm) and particles of spherical shape. Moreover, the silica adsorbents obtained manifested high activity. Their surface area reached values in the 340–390 m² g^?1 range.     

Toughening performance of glass fibre composites with core–shell rubber and silica nanoparticle modified matrices

The fracture energies of glass fibre composites with an anhydride-cured epoxy matrix modified using core–shell rubber (CSR) particles and silica nanoparticles were investigated. The quasi-isotropic laminates with a central 0°/0° ply interface were produced using resin infusion. Mode I fracture tests were performed, and scanning electron microscopy of the fracture surfaces was used to identify the toughening mechanisms.The composite toughness at initiation increased approximately linearly with increasing particle concentration, from 328 J/m² for the control to 842 J/m² with 15 wt% of CSR particles. All of the CSR particles cavitated, giving increased toughness by plastic void growth and shear yielding. However, the toughness of the silica-modified epoxies is lower as the literature shows that only 14% of the silica nanoparticles undergo debonding and void growth. The size of CSR particles had no influence on the composite toughness. The propagation toughness was dominated by the fibre toughening mechanisms, but the composites achieved full toughness transfer from the bulk.     

Particle size distribution control and related properties improvements of tungsten powders by fluidized bed jet milling

Fine grinding process of different particle size tungsten powders was carried out by fluidized bed jet milling. The results showed that the jet milling treatment caused deagglomeration of tungsten powders, which led to particles sufficient dispersion and narrow particle size distribution. Grinding gas pressure of 0.70 Mpa made the particles achieve high speed which promoted the particles collision contributing to particle dispersion and shape modification. For tungsten powder with particle size of 3 μm FSSS, a higher packing density with 5.54 g/cm³ was obtained, compared with the 3.71 g/cm³ of the original powder. For tungsten powder with particle size of 1 μm FSSS, the big agglomerates disappeared and the particle size distribution become narrower, while small aggregates about 2–3 μm still exist after the jet milling process. For tungsten powder with particle size of 5 μm and 10 μm FSSS, different medium diameter particle size and narrow particle size distribution of monodisperse tungsten powders can be produced by the optimized jet milling parameters. More important, the effective dispersion, favorable shape modification and precise classification have been achieved in the simple process.     

Influence of Eu substitution for Gd on the structure and photoluminescent properties of (Gd1−xEux)2Ti2O7 pyrochlore solid solutions

This paper presents a study of the synthesis and structural properties of the pyrochlore-type titanates (Gd_1?xEu_x)₂Ti₂O₇. Six compositions with 0 ≤ x ≤ 1 were prepared by solid-state reaction with thermal treatments at 1000 and 1200 °C under atmospheric pressure conditions. All the products were systematically characterized by X-ray powder diffraction (XRD), Raman spectroscopy, photoluminescence (PL) and photoluminescent excitation spectra (PLE). Structural refinements of X-ray powder diffraction data using Rietveld method show that all compounds of the (Gd_1?xEu_x)₂Ti₂O₇ solid solution crystallize in a pyrochlore structure. The lattice parameters increase linearly with increasing Eu content in agreement with Vegard's rule. PL spectra show that the characteristic peaks correspond to the f–f transition ⁵D₀–⁷F_J (J = 1, 2, 3 and 4) of Eu³⁺. The effect of Eu³⁺ ions concentration on the optical properties, namely, photoluminescence emission, is measured and discussed. The oxides exhibit higher PL intensity with the Eu³⁺ ion concentration and strong orange emission at 589 nm (⁵D₀–⁷F₁) corresponding to the magnetic dipole transition.     

Quantitative analysis on friction stress of hot-extruded AZ31 magnesium alloy at room temperature

Mg alloy AZ31 with ～79% (volume fraction of scattering less than 30°) basal-fiber texture through hot extrusion exhibits strong grain-size dependent yield strength. Samples with grain sizes varying from 4.5 to 22.3 μm were obtained by altering annealing time durations. The Hall-Petch relations of tension and compression are σ_0.2 = 86+200d^?1/2 and σ_0.2 = 17 + 327d^?1/2, respectively. Considering the correlation between grain orientation and deformation modes, a novel weighted average method of calculating friction stress σ₀ was proposed, and results of calculation agreed with the experimental ones, which can reasonably understand the yielding behavior in tension and compression.     

Ribbon-like and rod-like hydroxyapatite crystals deposited on titanium surface with electrochemical method

Homogeneous coatings were attained by electrochemical method in electrolytes containing Ca²⁺ and PO₄³⁻ ions with Ca/P ratio being 1.67. SEM observation showed that the hydroxyapatite (HAp,Ca₁₀(PO₄)₆(OH)₂) crystals prepared with higher concentration electrolyte (4 × 10^− 2 M Ca²⁺) are ribbon-like with thickness of nanometer size, a morphology seldom reported previously. In an electrolyte of lower concentration (6 × 10^− 4 M Ca²⁺), the HAp crystals formed are rod-like with a hexagonal cross section and diameter of about 70–80 nm. XRD patterns and IR spectra confirmed that the coatings consist of HAp crystals. TEM micrographs and SAD indicated that the longitude direction for both ribbon-like and rod-like crystal is [002], and the flat surface of the ribbon is (110). HRTEM showed that the ribbon-like crystal is a mixture of HAp and octacalcium phosphate (OCP, Ca₈H₂(PO₄)₆.5H₂O).