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At least 127 records · Page 7

Quaternary M{sub 0.25}Cu{sub 0.25}Mg{sub 0.5}Fe{sub 2}O{sub 4} (M = Ni, Zn, Co, Mn) ferrite oxides: Synthesis, characterization and magnetic properties

Highlights: • Superparamagnetic quaternary nanoferrite (M{sub 0.25}Cu{sub 0.25}Mg{sub 0.5}Fe{sub 2}O{sub 4,} where M = Mn, Zn, Co, Ni) were obtained. • C, O, H and metals were observed by XPS analysis. • Phases purity were confirmed by XRD diffraction and crystallite size (3–10 nm) were determind. - Abstract: We report the synthesis of M{sub 0.25}Cu{sub 0.25}Mg{sub 0.5}Fe{sub 2}O{sub 4} (where M = Mn, Zn, Co, Ni) nanoparticles using the coprecipitation method in the presence of carboxymethyl cellulose (CMC) as the in-situ surfactant. The crystalline structure and surface morphology were examined by means of X-ray diffraction (XRD) and scanning electron microscopy (SEM) and it was established that the average diameter of the magnetic nanoparticles (MNPs) is in the range of 3–10 nm. X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared spectroscopy (FTIR) show that the MNPs are activated by the hydrophilic groups of the surfactant, which coat them and enhance their stability. The vibrating sample magnetometry measurements show the superparamagnetic behavior of the nanoparticles. Due to their small crystallite size, which implies large surface area, and their functionalization with organic groups, the obtained nanoparticles could have medical and catalytic applications.

36 MATERIALS SCIENCE↗

Enhancement of three-photon near-infrared quantum cutting in β-NaYF4:Er3+ nanoparticles by Ag nanocubes

Highlights: • Three-photon near-infrared quantum cutting is obtained in β-NaYF{sub 4}:Er{sup 3+} NPs. • Quantum cutting efficiency as high as 242.59% is calculated from decay curves. • Plasmon-enhanced three-photon quantum cutting is achieved by Ag nanocubes. • The maximum quantum cutting enhancement factor reaches 2.86. - Abstract: The near-infrared (NIR) quantum cutting (QC) nanoparticles (NPs) β-NaYF{sub 4}:Er{sup 3+} are prepared by coprecipitation method. Three-photon NIR QC luminescence at 1520 nm ({sup 4}I{sub 13/2} → {sup 4}I{sub 15/2}) is obtained under the excitation of 519 nm ({sup 4}I{sub 15/2} → {sup 2}H{sub 11/2}). The corresponding QC efficiency η{sub QC} calculated from the luminescence decay curves reaches as 242.59%. Furthermore, three-photon NIR QC luminescence is enhanced by the localized surface plasmon resonance of Ag nanocubes (NCs). The influence of Ag NCs concentration on three-photon QC luminescence is investigated, and the results show that the optimal concentration of Ag NCs is 0.10% with the enhancement factor reached a maximum as 2.86. Our study may have potential application as a QC layer to improve the photovoltaic conversion efficiency of germanium (Ge) solar cells.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Influence of high energy ball milling on structural parameters, cation distribution and magnetic enhancement of nanosized Co0.3Zn0.7Fe2O4

Highlights: • Magnetic enhancement in mechanically activated nanosized Co{sub 0.3}Zn{sub 0.7}Fe{sub 2}O{sub 4} ferites. • Influence of crystal structure, cation distribution and stress anisotropy on magnetic and hyperfine properties. • A simple method for estimation of cation distribution of ferrites has been proposed. • Probing core-shell type magnetic structure of ferrite nanoparticles by infield Mössbauer and dc magnetic measurement. • Memory effect in the dc magnetization. - Abstract: Herein, we report the role of mechanical activation in modifying the structural, microstructural, magnetic and hyperfine parameters of nanosized Co{sub 0.3}Zn{sub 0.7}Fe{sub 2}O{sub 4} having average particle size ∼16.6 nm synthesized via coprecipitation method followed by high energy ball milling with cation distribution (Zn{sup 2+}{sub 0.61}Fe{sup 3+}{sub 0.39}){sub A} [Co{sup 2+}{sub 0.3}Zn{sup 2+}{sub 0.09}Fe{sup 3+}{sub 1.61}]{sub B}O{sub 4}. The values of the blocking temperature and Curie temperature of the sample are 220 and 270 K, respectively. The values of saturation magnetization at 300 and 5 K are 59 and 88 emu g{sup −1}and those of the coercivity at 100 and 5 K are 400 and 5000 Oe, respectively. The values of the magnetic parameters of the sample are greater than those of its counterparts synthesized by chemical methods. A model for precise estimation of the cation distribution of ferrites has been proposed. Moreover, the memory effect obtained in the dc magnetization of the sample can be used for generating, storing and retrieving binary bit pattern.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

ZnCr-LDH/N-doped graphitic carbon-incorporated g-C3N4 2D/2D nanosheet heterojunction with enhanced charge transfer for photocatalysis

Highlights: • Synthesize a novel ZnCr-LDH/modified-g-C{sub 3}N{sub 4} photocatalyst by a facile template free in situ coprecipitation method approach. • The synergistic effect of adsorption and catalytic improve the ability of photodegradation. • Composites with 2D-2D nanosheets structure present superior catalytic activity than pure phases. • Calcinated photocatalyst has high visible-light respond capacity and low recombination rate of electron-hole pairs due to the formation of heterojunction. - Abstract: In this work, we successfully synthesized a novel ZnCr-LDH/N-doped graphitic carbon-incorporated g-C{sub 3}N{sub 4} (g-C{sub 3}N{sub 4}-C(N)) hybrid with unique two-dimensional/two-dimensional (2D-2D) structure for the efficient degradation of Congo red under visible light irradiation. It was demonstrated that ZnCr-LDH/g-C{sub 3}N{sub 4}-C(N) exhibited lower photogenerated electron-hole recombination rate and enhanced light harvesting. Furthermore, its derived calcined product also showed outstanding performance due to the unique heterogeneous structure and the synergistic effect between photocatalysis and adsorption. In addition, the mixed metal oxide ZnO and ZnCr{sub 2}O{sub 4} in ZnCr-CLDH/g-C{sub 3}N{sub 4}-C(N) dispersed uniformly on the g-C{sub 3}N{sub 4}-C(N) exposed more active sites and facilitated the photodegradation of pollutants.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Recovery of yttrium from fluorescent powder of cathode ray tube, CRT: Zn removal by sulphide precipitation

Highlights: • Treatment of fluorescent powder of CRT waste. • Factorial experimental designs to study acid leaching of fluorescent powder and the purification of leach liquors. • Recover of yttrium by precipitation using oxalic acid. • Suitable flowsheet to recover yttrium from fluorescent powder. - Abstract: This work is focused on the recovery of yttrium and zinc from fluorescent powder of cathode ray tube (CRT). Metals are extracted by sulphuric acid in the presence of hydrogen peroxide. Leaching tests are carried out according to a 2{sup 2} full factorial plan and the highest extraction yields for yttrium and zinc equal to 100% are observed under the following conditions: 3 M of sulphuric acid, 10% v/v of H{sub 2}O{sub 2} concentrated solution at 30% v/v, 10% w/w pulp density, 70 °C and 3 h of reaction. Two series of precipitation tests for zinc are carried out: a 2{sup 2} full factorial design and a completely randomized factorial design. In these series the factors investigated are pH of solution during the precipitation and the amount of sodium sulphide added to precipitate zinc sulphide. The data of these tests are used to describe two empirical mathematical models for zinc and yttrium precipitation yields by regression analysis. The highest precipitation yields for zinc are obtained under the following conditions: pH equal to 2–2.5% and 10–12% v/v of Na{sub 2}S concentrated solution at 10% w/v. In these conditions the coprecipitation of yttrium is of 15–20%. Finally further yttrium precipitation experiments by oxalic acid on the residual solutions, after removing of zinc, show that yttrium could be recovered and calcined to obtain the final product as yttrium oxide. The achieved results allow to propose a CRT recycling process based on leaching of fluorescent powder from cathode ray tube and recovery of yttrium oxide after removing of zinc by precipitation. The final recovery of yttrium is 75–80%.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Structural, Electrochemical, and (De)lithiation Mechanism Investigation of Cation-Disordered Rocksalt and Spinel Hybrid Nanomaterials in Lithium-Ion Batteries

Significant demand for lithium-ion batteries necessitates alternatives to Co- and Ni-based cathode materials. Cation-disordered materials using earth-abundant elements are being explored as promising candidates. Here, in this paper, we demonstrate a coprecipitation synthetic approach that allows direct preparation of disordered rocksalt Li 2.4 Fe 1.0 Ti 1.0 O 4.7 (r-LFTO·C) and spinel structured hybrid Li 0.5 Fe 1.0 Ti 0.9 O 3.2 ·C (s-LFTO·C) nanoparticles with a conformal conductive carbon coating. High-angle annular dark-field imaging coupled with electron energy loss spectroscopy mapping shows uniform Fe/Ti distribution with minor compositional variation among particles. Cation disorder was confirmed for both of the materials at an atomic level, with a short-range order more pronounced in r-LFTO·C. Operando X-ray absorption spectroscopy, ex situ hard X-ray photoelectron spectroscopy, ex situ soft X-ray absorption spectroscopy, and ex situ synchrotron X-ray diffraction were used to investigate (de)lithiation in the bulk and at the surface. Structurally, the r-LFTO·C demonstrated reversible partial Fe center migration between octahedral and tetrahedral sites during (de)lithiation. The r-LFTO·C evidenced that the redox of O was coincident with iron redox during initial electrochemical cycling, while iron redox dominated later cycling. In contrast, s-LFTO·C electrochemistry involved iron redox throughout the cycling process. The findings rationalize the differences in the electrochemistry where r-LFTO·C shows higher initial capacity yet poorer capacity retention over a voltage window where O redox can be accessed, while the s-LFTO·C shows lower initial capacity yet improved capacity retention.

25 ENERGY STORAGE↗

Study of de-watering from the gelatinous precipitate formed during co-precipitation of Nd-YAG powder

Neodymium doped Yttrium Aluminium Garnet (Nd:YAG) ceramics have been synthesised using coprecipitation technique and high temperature vacuum sintering. Gelatinous like precipitates were obtained when precursors of Nd, Al and Yb-nitrate solutions are co-precipitated using ammonia co-precipitant. De-watering from the gelatinous like precipitates is a big challenge and it possesses difficulty in filtration. Evaporation of water by heating resulted in strong agglomerated powder. Different agents were used to ease the filtration process, which is correlated with the phase in the calcined powder.

36 MATERIALS SCIENCE↗

Structural and dielectric properties of Nd/Ca co-doped bi-ferrite multiferroics

Single-phase polycrystalline samples of Bi{sub 0.8}Nd{sub 0.2−x}Ca{sub x}FeO{sub 3} (x = 0.0, 0.1) were synthesized by chemical coprecipitation method. X-ray diffraction patterns accompanied by Rietveld-refined crystal structure parameters reveal the phase transition of Bi{sub 0.8}Nd{sub 0.1}Ca{sub 0.1}FeO{sub 3} with rhombohedral R3c symmetry to triclinic structure of Bi{sub 0.8}Nd{sub 0.2}FeO{sub 3} sample. Frequency dependence of dielectric constant (ε') and dielectric loss (tanδ), infers enhancement of both ε' (tanδ) in narrow band gap of Nd/Ca co-doped BFO as compare to wide band pristine BFO.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Thermoluminescence of nanocrystalline CaSO{sub 4}: Dy for gamma dosimetry and calculation of trapping parameters using deconvolution method

Nanorods of CaSO{sub 4}: Dy having diameter 20 nm and length 200 nm have been synthesized by the chemical coprecipitation method. These samples were irradiated with gamma radiation for the dose varying from 0.1 Gy to 50 kGy and their TL characteristics have been studied. TL dose response shows a linear behavior up to 5 kGy and further saturates with increase in the dose. A Computerized Glow Curve Deconvolution (CGCD) program was used for the analysis of TL glow curves. Trapping parameters for various peaks have been calculated by using CGCD program.

61 RADIATION PROTECTION AND DOSIMETRY↗

Modulated magnetoelectric property of BiFeO{sub 3} incorporated in Co{sub 0.50}Fe{sub 0.50}Fe{sub 2}O{sub 4}

Nanocomposite of (BiFeO{sub 3}){sub 0.50} (Co{sub 0.50}Fe{sub 0.50}Fe{sub 2}O{sub 4}){sub 0.50} were prepared by using a chemical coprecipitation method. X- ray diffraction (XRD) was recorded to confirm the desired crystallographic phase of the sample. The nanocrystallite size of each component including their average size was calculated from the broadening of the XRD peaks using the well known Debye-Scherrer equation. To confirm the presence of the onset of magnetic ordering in ac hysteresis loops were recorded. The dielectric and ferroelectric property was also confirmed the presence of electric ordering in the sample at room temperature. The magnetic property of BFO has been substantially enhanced by the strong magnetic host of Co{sub 0.50}Fe{sub 0.50}Fe{sub 2}O{sub 4}.

36 MATERIALS SCIENCE↗

Milling time and temperature dependence on Fe{sub 2}TiO{sub 5} nanoparticles synthesized by mechanical alloying method

Fe{sub 2}TiO{sub 5} is one type of titanate oxides which has M{sub x}Ti{sub y}O{sub z} crystal structure. It has various kinds of applications due to its electric and magnetic properties such as spintronics, electromagnetic devices, and gas sensor. In this study, Fe{sub 2}TiO{sub 5} nanoparticles were synthesized by simple mechanical alloying using planetary ball milling machine with various milling times and sintering temperatures. TiO{sub 2} and Fe{sub 2}O{sub 3} powders obtained from coprecipitation process were used as starting materials. The resulted Fe{sub 2}TiO{sub 5} powders were characterized by X-Ray Diffraction (XRD), Scanning Electron Microscopy (SEM), and Vibration Sample Magnetometer (VSM) in order to observe crystal quality, particles morphology, and magnetic properties respectively. As the milling time increases and the sintering temperature decreases, the crystal size of Fe{sub 2}TiO{sub 5} phase decreases. The smallest crystal size of the synthesized Fe{sub 2}TiO{sub 5} nanoparticles was ∼ 51 nm obtained by the milling time of 25 hours and sintering at 1100°C. The distribution of the resulted Fe{sub 2}TiO{sub 5} nanoparticles was not so homogeneous due to the appearance of small amount impurities. The VSM measurements show that a paramagnetic property was observed which should be analyzed more details on the low external magnetic fields.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Synthesis and characterization of black, red and yellow nanoparticles pigments from the iron sand

The aim of this research is to synthesize nanoparticles of black pigment of Magnetite (Fe{sub 3}O{sub 4}), red pigment of hematite (α-Fe{sub 2}O{sub 3}), and yellow pigment of ghoetite (α-FeOOH) from the iron sand. The black pigment of Fe{sub 3}O{sub 4} and the yellow pigment α-FeOOH nanoparticles were synthesized by coprecipitation method with variation of pH. Whereas, the red pigment Fe{sub 2}O{sub 3} was synthesized by sintering Fe{sub 3}O{sub 4} nanoparticles at temperature between 400 °C and 700 7°C for 1 hour. All the pigments has been characterized using X-ray diffraction and SEM. The XRD results shown that the particle size of the black pigmen Fe{sub 3}O{sub 4}, red pigment Fe{sub 3}O{sub 4} and yellow pigment α-FeOOH are around 12, 32, and 30 nm respectively. The particle size of Fe{sub 2}O{sub 3} nanoparticles increase by increasing sintering temperature from 32 nm at 400 °C to 39 nm at 700 °C. For yellow pigment of α-FeOOH, the particle size increase by increasing pH from 30,54 nm at pH 4 to 48,60 nm at pH 7. The SEM results shown that the morphologies of black, yellow and red pigments are aglomarated.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Multicolour upconversion emission from Ho{sup 3+}-Tm{sup 3+}-Yb{sup 3+} codoped CaMoO{sub 4} phosphor

The Ho{sup 3+}-Tm{sup 3+}-Yb{sup 3+} codoped CaMoO4 phosphor powder has been synthesized by chemical coprecipitation technique. For the structural investigation the X-ray diffraction analysis has been done. Multicolour upconversion (UC) emission in the visible region from the prepared material has been observed under the 980 nm near infrared (NIR) excitation. The UC emission bands ∼ 474 nm (blue), ∼ 541 nm (green) and ∼ 661 nm (red) region have been assigned as {sup 1}G{sub 4}→{sup 3}H{sub 6} (Tm{sup 3+}), {sup 5}F{sub 4}{sup 5}S{sub 2}→{sup 5}I{sub 8} (Ho{sup 3+}) and {sup 5}F{sub 5}→{sup 5}I{sub 8} (Ho{sup 3+}) transitions respectively.

36 MATERIALS SCIENCE↗

Structural and FMR lineshape analysis of Mn Zn-ferrite nanoparticles

The Mn{sub 0.25}Zn{sub 0.75}Fe{sub 2}O{sub 4} (MZF) nanoparticles of 3 to 5 nm size were synthesized by chemical coprecipitation method. The X-ray diffraction (XRD) patterns were well fitted with single phase spinel ferrite structure using Rietveld analysis as Fd-3m space group. The ferromagnetic resonance (FMR) spectra of MZF nanoparticles becomes more asymmetric with increase in particle size from 3 to 5 nm. The change in FMR line shape is attributed to the increase in ferromagnetic interactions and anisotropy in the system with increase in nanoparticles size. The decrease in total absorption of the FMR line with decreasing temperature at low temperatures indicates weak antiferromagnetic coupling between the octahedral and tetrahedral sublattices of the spinel ferrite system.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Electrostatic vs steric stabilization of Fe{sub 3}O{sub 4} and Co{sub 0.5}Fe{sub 2.5}O{sub 4} nanoparticles

Magnetic nanoparticles of magnetite/maghemite and cobalt ferrite Co{sub 0.5}Fe{sub 2.5}O{sub 4} were stabilized in deionized water with perchloric acid and, respectively, sodium oleate in order to prevent agglomeration and sedimentation tendency aiming further biomedical applications. Results obtained through Scanning Electron Microscopy (SEM), X-ray Diffraction (XRD), Nanoparticle Tracking Analysis (NTA), and Vibrating Sample Magnetometry (VSM) were discussed comparatively for the four suspensions highlighting specific microstructural and magnetic features of each type of soft magnetic colloidal nanomaterial on the background of coprecipitation method adjusting. The results entitled us to plan in the next research stage biological tests focused on such nanoparticle suspensions impact on cell cultures.

36 MATERIALS SCIENCE↗

Influence of pH on the formulation of TiO{sub 2} powder prepared by co-precipitation of TiCl{sub 3} and photocatalytic activity

Titanium dioxide (titania) nanoparticle were synthesized by coprecipitation process of titanium trichloride (TiCl{sub 3}) in aqueous medium, with NH{sub 4}OH as pH regulator. The pH solution was varied during the synthesis process between pH 3-8.4, and all samples were calcined temperature at 400°C for 3 hours. Characteristics and properties of the TiO{sub 2} powder were investigated using X-ray diffraction (XRD), Scanning Electron Microscopy (SEM). XRD results show that the single-phase rutile formed when the pH is less than 5, anatase single phase formed began pH 8, and the pH of the solution between 5-8 formed mixed phase rutile-anatase-brookite, rutile-brookite or anatase-brookite. Methylene Blue (MB) photodegradation test were performed in order to evaluate photocatalytic activity. Nanoparticles TiO{sub 2} rutile, anatase phase, and mixed phase rutile-brookite, anatase-brookite used to test the photocatalytic activity by measuring the absorbance spectrum photodegradation using UV-Vis spectrometer. The test results showed that the mixture phase of rutile-brookite provide the greatest photodegradation than other phases.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Synthesis of nano-forsterite powder by making use of natural silica sand

Nano-forsterite powder with natural silica sand and magnesium powder as the raw materials have been succesfully synthesized. The silica sand was purified followed by a coprecipitation process to obtain colloidal silica. The magnesium powder was dissolved in a chloric acid solution to obtain MgCl{sub 2} solution. The nanoforsterite powder was synthesised using a sol-gel method which included the mixing the colloidal silica and the MgCl{sub 2} solution with various aging and filtering processes. The samples were dried at 100 °C using a hot plate and then the dried powders were calcinated at 900 °C for 2 hours. The samples were characetised for their elements and phase compositions using X-ray Flourescence (XRF) and X-ray Diffraction (XRD) methods, respectively. The diffraction data were qualitatively analyzed using Match!2 software and quantitatively using Rietica software. The crystallite size was verified using Transmission Electron Microscopy (TEM). Results of XRD data analysis showed that the forsterite content reached up to 90.5% wt. The TEM average crystallite size was approximately 53(6) nm.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Effect of calcination temperature on the photocatalytic activity of TiO{sub 2} powders prepared by co-precipitation of TiCl{sub 3}

The adsorption of basic dye methylene blue (MB) onto titanium dioxide (titania) powder that were prepared by coprecipitation method of TiCl{sub 3} and NH{sub 4}OH as iniatial material with different calcination temperature was studied to examine the photocatalytic activity. Synthesis process carried out by the solution pH was adjusted to be 8. Effect of calcination temperature on the titania powder were characterized with Differential Scanning Calorimetry/Thermogravimetry (DSC/TG), X-ray diffraction (XRD), and Scanning Electron Microscopy (SEM). The result of TG and XRD showed that the NH{sub 4}Cl decomposed between 235-372°C. The XRD result showed that the anatase TiO{sub 2} only contained a single phase when the calcination temperature of the precursor at 800°C, and over which it began to grow rutile phase. The influence of synthesis condition on the photocatalytic activity of TiO{sub 2} powder was determined by the photodegradation of MB dye under UV light.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗