Simple and low-temperature synthesis of NiO nanoparticles through solid-state thermal decomposition of the hexa(ammine)Ni(II) nitrate, [Ni(NH3)6](NO3)2, complex

NiO nanoparticles with an average size of about 12 nm were easily prepared via the thermal decomposition of hexa(ammine)Ni(II) nitrate complex, [Ni(NH₃)₆](NO₃)₂, at low temperature of 250 °C. The product was characterized by thermal analysis (TGA/DTA), X-ray diffraction (XRD), Fourier-transformed infrared spectroscopy (FT-IR), UV-Vis spectroscopy, BET specific surface area measurement, scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM), and magnetic measurement. The magnetic measurement revealed a small hysteresis loop at room temperature, confirming a superparamagnetic (weak ferromagnetic) nature of the synthesized NiO nanoparticles. Indeed, the NiO nanoparticles prepared by this method could be an appropriate semiconductor material due to the optical band gap of 3.35 eV which shows a red shift in comparison with the previous reports. This method is simple, fast, safe, low-cost and also suitable for industrial production of high purity NiO nanoparticles for applied purposes.     

Preparation and characterization of pure single-phase BiFeO3 nanoparticles through thermal decomposition of the heteronuclear Bi[Fe(CN)6]·5H2O complex

The heteronuclear Bi[Fe(CN)₆]·5H₂O complex was synthesized and single-phase perovskite-type BiFeO₃ nanoparticles with an average size of 30 nm were obtained by its decomposition at 600 °C. The complex and its decomposition products were analyzed using elemental analysis, thermal analysis (TGA/DTA/DSC), X-ray diffraction (XRD), Fourier-transformed infrared spectroscopy (FT-IR), UV–Vis spectroscopy, BET specific surface area measurement, scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS) and magnetic measurements. The magnetic measurement confirms that the product shows a ferromagnetic order at room temperature, which may be ascribed to the size confinement effect. The DTA and DSC results confirm the multiferroic nature of the BiFeO₃ nanoparticles with Neel and Curie points at 372 and 825 °C, respectively. The BiFeO₃ prepared by this method could be an appropriate visible-light photocatalytic material due to its strong absorption band in the visible region. This method is simple, low-cost, safe and also suitable for industrial production of high purity perovskite-type BiFeO₃ nanoparticles for electromagnetic applications.     

Synthesis and characteristic of the Fe3O4@SiO2@Eu(DBM)3·2H2O/SiO2 luminomagnetic microspheres with core-shell structure

The core-shell structured luminomagnetic microsphere composed of a Fe₃O₄ magnetic core and a continuous SiO₂ nanoshell doped with Eu(DBM)₃·2H₂O fluorescent molecules was fabricated by a modified Stöber method combined with a layer-by-layer assembly technique. X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), confocal microscopy, photoluminescence (PL), and superconducting quantum interface device (SQUID) were employed to characterize the Fe₃O₄@SiO₂@Eu(DBM)₃·2H₂O/SiO₂ microspheres. The experimental results show that the microshpere has a typical diameter of ca. 500 nm consisting of the magnetic core with about 340 nm in diameter and silica shell doped with europium complex with an average thickness of about 80 nm. It possesses magnetism with a saturation magnetization of 25.84 emu/g and negligible coercivity and remanence at room temperature and exhibits strong red emission peak originating from electric-dipole transition ⁵D₀ → ⁷F₂ (611 nm) of Eu³⁺ ions. The luminomagnetic microspheres can be uptaken by HeLa cells and there is no adverse cell reaction. These results suggest that the luminomagnetic microspheres with magnetic resonance response and fluorescence probe property may be useful in biomedical imaging and diagnostic applications.     

Hydrothermal synthesis of cobalt carbonates using different counter ions: An efficient precursor to nano-sized cobalt oxide (Co3O4)

Synthesis of submicrometer crystalline particles of cobalt carbonate was achieved hydrothermally using different cobalt salts and urea with a molar ratio from 1:3 to 1:20 (cobalt salt:urea) in aqueous solutions at 160 °C for 24-36 h, in the presence of cetyltrimethylammonium bromide (CTAB) as a surfactant. Nanoparticles of Co₃O₄, with an average size from 30 to 39 nm, were obtained by thermal decomposition of CoCO₃ samples at 500 °C for 3 h in an electrical furnace. The as-synthesized products were characterized by powder X-ray diffraction (XRD), Fourier transform infrared spectra (FT-IR), transmission electron microscopy (TEM), scanning electron microscopy (SEM), UV-Vis spectra and thermal analysis. Studying the optical properties of the as-prepared cobalt oxide nanoparticles showed the presence of two band gaps, the values of which confirmed the semiconducting properties of the prepared Co₃O₄.     

A simple route to synthesize nanocrystalline nickel ferrite (NiFe2O4) in the presence of octanoic acid as a surfactant

Nanocrystalline nickel ferrite (NiFe₂O₄) powder was prepared by a co-precipitation method from Ni and Fe chlorides. The as-prepared samples were characterized by powder X-ray diffractometry (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FT-IR) and vibrating sample magnetometry (VSM). SEM and TEM indicated that the particles were spherical with particle sizes in the range 25 ± 5 nm. The magnetic properties of the sample were measured by using a vibrating sample magnetometer, which showed that the sample exhibited typical ferromagnetic behavior at room temperature, while a finite coercivity of 245.5 Oe was present at 300 K. The saturation magnetization of the sample (23.13 emu/g) was significantly lower than that for the reported multidomain bulk particles (55 emu/g), reflecting the ultrafine nature of the sample.     

Thermal decomposition route for synthesis of Mn3O4 nanoparticles in presence of a novel precursor

The synthesis of manganese oxide (Mn₃O₄) nanoparticles by using thermal decomposition and its physicochemical characterization are being reported in present investigation. As a new precursor, [bis(2-hydroxy-1-naphthaldehydato)manganese(II)] complex was used in the presence of oleylamine (C₁₈H₃₇N) as both surfactant and solvent to control the size of resulting nanoparticle. The products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) spectroscopy, thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS) and Raman spectrum. Synthesized manganese oxide nanoparticles have a tetragonal structure with average size of 9–24 nm. The phase pure samples were characterized by using X-ray photoelectron spectroscopy (XPS) for Mn 2p level. The values of binding energies are consistent with the relative values are reported in the literature. As a comparison between two methods, the novel precursor thermally was treated in solid state reaction in different temperature, 400, 500, and 600 °C and the products were characterized by SEM images. Magnetic property of the as-prepared Mn₃O₄ nanoparticle shows a ferromagnetic behavior with high saturation magnetization and coercivity.     

Synthesis of nano-sized crystalline oxide ion conducting fluorite-type Y2O3-doped CeO2 using perovskite-like BaCe0.9Y0.1O2.95 (BCY) and study of CO2 capture properties of BCY

Formation of nano-sized Y₂O₃-doped CeO₂ (YCO) was observed in the chemical reaction between proton conducting Y₂O₃-doped BaCeO₃ (BCY) and CO₂ in the temperature range 700-1000 °C, which is generally prepared by wet-chemical methods that include sol-gel, hydrothermal, polymerization, combustion, and precipitation reactions. BCY can capture CO₂ of 0.13 g per ceramic gram at 700 °C, which is comparable to that of the well-known Li₂ZrO₃ (0.15 g per ceramic gram at 600 °C). Powder X-ray diffraction (PXRD), energy dispersive X-ray analysis (EDX), laser particle size analysis (LPSA), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and ac impedance spectroscopy were employed to characterize the reaction product obtained from reaction between BCY and CO₂ and subsequent acid washing. PXRD study reveals presence of fluorite-like CeO₂ (a=5.410 (1) Å) structure and BaCO₃ in reaction products. TEM investigation of the acid washed product showed the formation of nano-sized material with particle sizes of about 50 nm. The electrical conductivity of acid washed product (YCO) in air was found to be about an order higher than the undoped CeO₂ reported in the literature.     

Synthesis and characterization of NixMg1−xAl2O4 nano ceramic pigments via a combustion route

MgAl₂O₄ was successfully used as a crystalline host network for the synthesis of nickel-based nano cyan refractory ceramic pigments. Different compositions of Ni_xMg_1−xAl₂O₄ (0.1 ? x ? 0.8) powders have been prepared by using a low temperature combustion reaction (LTCR) of the corresponding metal nitrates with urea (U) as a fuel at 300 °C in an open air furnace. The as-synthesized samples were characterized by thermal analysis (TG-DTG/DTA), X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and transmission electron microscopy (TEM). UV-Vis and diffuse reflectance spectroscopy (DRS) using CIE- L^∗a^∗b^∗ parameters methods have been used for color measurements. The results show that the Ni_xMg_1−xAl₂O₄ samples are the crystalline phase with a particle size of 8.85-43.66 nm in the temperature range 500-1200 °C. The density, particle size, shape and color are determined for all the prepared samples with different calcination times and temperatures.     

Photocatalytic activity of ZrO2 nanoparticles prepared by electrical arc discharge method in water

ZrO₂ nanoparticles were synthesized through arc discharge of zirconium electrodes in deionized (DI) water. X-ray diffraction (XRD) analysis of the as prepared nanoparticles indicates formation a mixture of nanocrystalline ZrO₂ monoclinic and tetragonal phase structures. Transmission electron microscopy (TEM) images illustrate spherical ZrO₂ nanoparticles with 7–30 nm diameter range, which were formed during the discharge process with 10 A arc current. The average particle size was found to increase with the increasing arc current. X-ray photoelectron spectroscopy (XPS) analysis confirms formation of ZrO₂ at the surface of the nanoparticles. Surface area of the sample prepared at 10 A arc current, measured by BET analysis, was 44 m²/g. Photodegradation of Rhodamine B (Rh. B) shows that the prepared samples at lower currents have a higher photocatalytic activity due to larger surface area and smaller particle size.     

Symmetry of LaAlO3 nanocrystals as a function of crystallite size

Properties of LaAlO₃ nanocrystallites obtained by the precipitation method, doped with praseodymium and chromium ions were examined by spectroscopic means. Raman spectroscopy, high resolution transmission electron microscopy (HRTEM), X-ray diffraction (XRD) and electronic spectroscopy proved that symmetry of LaAlO₃ crystallites depends on their size. At room temperature the smallest obtained crystals (average size ∼5 nm) have cubic symmetry, while the largest ones (average size over 110 nm) exhibit rhombohedral symmetry. Possible explanations for this phenomenon are discussed.     

Hydrophilic and hydrophobic nano-sized Mn3O4 particles

Mn₃O₄ Hausmanite nanoparticles were prepared in aqueous solution by using metallic salt and hydrazine as precursor and reducing agent, respectively. The crystallite sizes ranged from 10 to 20 nm and the particle diameter distribution was very narrow and estimated between 20 and 30 nm. Influence of some parameters such as temperature, time of reaction, surfactant nature was studied for a synthesis in an aqueous medium. The as-made manganese oxides particles could be dispersed in an organic solvent containing stabilizing agents, according to perform the synthesis in an H₂O/n-hexan two-phase medium. These nanoparticles were characterized by X-ray diffraction, infrared spectroscopy, scanning and transmission electron microscopies and nitrogen absorption measurements.     

Fe3O4/PEI/Au@CdSe/CdS多功能复合材料的制备与表征

以共沉淀法制备出Fe₃O₄纳米粒子,通过聚乙烯亚胺(PEI)修饰Fe₃O₄纳米粒子,再原位复合上Au纳米粒子,制得Fe₃O₄/PEI/Au纳米颗粒微球。再将Fe₃O₄/PEI/Au纳米颗粒与巯基乙酸修饰的量子点CdSe/CdS连接,成功制备了Fe₃O₄/PEI/Au@CdSe/CdS多功能复合微球。经过傅里叶变换红外光谱仪(FTIR)、荧光分光光度计、荧光显微镜、X射线衍射(XRD)、透射电子显微镜(TEM)及振动样品磁强计(VSM)的表征。结果表明:多功能复合微球的粒径在40 nm左右,具有超顺磁性,剩磁,矫顽力近似等于零,饱和磁化强度为28.83 A·m²·kg^-1,同时兼有优越的荧光性能和金纳米粒子的特性。     

Fe3O4/PEI/Au@CdSe/CdS多功能复合材料的制备与表征

以共沉淀法制备出Fe₃O₄纳米粒子,通过聚乙烯亚胺(PEI)修饰Fe₃O₄纳米粒子,再原位复合上Au纳米粒子,制得Fe₃O₄/PEI/Au纳米颗粒微球。再将Fe₃O₄/PEI/Au纳米颗粒与巯基乙酸修饰的量子点CdSe/CdS连接,成功制备了Fe₃O₄/PEI/Au@CdSe/CdS多功能复合微球。经过傅里叶变换红外光谱仪(FTIR)、荧光分光光度计、荧光显微镜、X射线衍射(XRD)、透射电子显微镜(TEM)及振动样品磁强计(VSM)的表征。结果表明:多功能复合微球的粒径在40nm左右,具有超顺磁性,剩磁,矫顽力近似等于零,饱和磁化强度为28.83A·m₂·kg^-1,同时兼有优越的荧光性能和金纳米粒子的特性。     

Synthesis, crystal structures and photoluminescence properties of new oxyborates, Mg5NbO3(BO3)3 and Mg5TaO3(BO3)3, with novel warwickite-type superstructures

Single crystals of new oxyborates, Mg₅NbO₃(BO₃)₃ and Mg₅TaO₃(BO₃)₃, were prepared at 1370 °C in air using B₂O₃ as a flux. They were colorless and transparent with block shapes. X-ray diffraction analysis of the single crystals revealed Mg₅NbO₃(BO₃)₃ and Mg₅TaO₃(BO₃)₃ to be isostructural. The X-ray diffraction reflections were indexed to the orthorhombic Pnma (No. 62) system with a=9.3682(3) Å, b=9.4344(2) Å, c=9.3379(3) Å and Z=4 for Mg₅NbO₃(BO₃)₃ and a=9.3702(3) Å, b=9.4415(3) Å, c=9.3301(2) Å and Z=4 for Mg₅TaO₃(BO₃)₃. The crystal structures of Mg₅NbO₃(BO₃)₃ and Mg₅TaO₃(BO₃)₃ are novel warwickite-type superstructures having ordered arrangements of Mg and Nb/Ta atoms. Polycrystals of Mg₅NbO₃(BO₃)₃ prepared by solid state reaction at 1200 °C in air showed broad blue-to-green emission with a peak wavelength of 470 nm under 270 nm ultraviolet excitation at room temperature.     

Synthesis and characterization of poly(vinyl phosphonic acid) (PVPA)-Fe3O4 nanocomposite

Poly(vinyl phosphonic acid) (PVPA)-Fe₃O₄ nanocomposite is synthesized by the precipitation of Fe₃O₄ in the presence of PVPA. Structural, surface, morphological, thermal properties and conductivity characterization/evaluation of the nanocomposite were performed by XRD, FT-IR, TEM, TGA and conductivity measurements respectively. The capping of PVPA around the Fe₃O₄ nanoparticles was confirmed by FT-IR spectroscopy, the interaction being via bridging oxygens of the phosphate and the nanoparticle surface. The crystallite and particle size were obtained as 6 ± 2 and 8.7 ± 0.1 nm from XRD line profile fitting and TEM image analysis respectively, which reveal nearly single crystalline nature of the Fe₃O₄ nanoparticles. Magnetic characterization of the bulk magnetite and (PVPA)-Fe₃O₄ nanocomposite reveals that both are in the superparamagnetic state at room temperature. The average magnetic domain size of the nanoparticles has been calculated using the Langevin function, which was fitted to the measured M-H hysteresis curves as 7.6 nm for the nanocomposite. In the nanocomposite, the reduction is due to the adsorption of PVPA onto the magnetite surface, which cancels some of the free spins at the surface causing a magnetically dead layer. Analysis of the conductivity and permittivity measurements revealed the coupling of ionic and polymer segmental motions and strong temperature dependency in the nanocomposite.     

Nickel(IV) dithiocarbamato complexes of the [Ni(ndtc)3]X type: X-ray structure of [Ni(hmidtc)3][FeCl4]

A series of fourteen octahedral nickel(IV) dithiocarbamato complexes of the general formula [Ni(ndtc)₃]X·yH₂O {ndtc stands for the appropriate dithiocarbamate anion, X stands for ClO₄⁻ (1-8; y = 0) or [FeCl₄]⁻ (9-14; y = 0 for 9-12, 1 for 13 and 0.5 for 14} was prepared by the oxidation of the corresponding nickel(II) complexes, i.e. [Ni(ndtc)₂], with NOClO₄ or FeCl₃. The complexes, involving a high-valent Ni^IVS₆ core, were characterized by elemental analysis (C, H, N, Cl and Ni), UV-Vis and FTIR spectroscopy, thermal analysis and magnetochemical and conductivity measurements. The X-ray structure of [Ni(hmidtc)₃][FeCl₄] (9) was determined {it consists of covalently discrete complex [Ni(hmidtc)₃]⁺ cations and [FeCl₄]⁻ anions} and this revealed slightly distorted octahedral and tetrahedral geometries within the complex cations, and anions, respectively. The Ni(IV) atom is six-coordinated by three bidentate S-donor hexamethyleneiminedithiocarbamate anions (hmidtc), with Ni-S bond lengths ranging from 2.2597(5) to 2.2652(5) Å, while the shortest Ni···Cl and Ni···Fe distances equal 4.1043(12), and 6.2862(6) Å, respectively. Moreover, the formal oxidation state of iron in [FeCl₄]⁻ as well as the coordination geometry in its vicinity was also proved by ⁵⁷Fe Mössbauer spectroscopy in the case of 9.     

Effect of capping and particle size on Raman laser-induced degradation of γ-Fe2O3 nanoparticles

Diol capped γ-Fe₂O₃ nanoparticles are prepared from ferric nitrate by refluxing in 1,4-butanediol (9.5 nm) and 1,5-pentanediol (15 nm) and uncapped particles are prepared by refluxing in 1,2-propanediol followed by sintering the alkoxide formed. X-ray diffraction (XRD) shows that all the samples have the spinel phase. Raman spectroscopy shows that the samples prepared in 1,4-butanediol and 1,5-pentanediol and 1,2-propanediol (sintered at 573 and 673 K) are γ-Fe₂O₃ and the 773 K-sintered sample is Fe₃O₄. Raman laser studies carried out at various laser powers show that all the samples undergo laser-induced degradation to α-Fe₂O₃ at higher laser power. The capped samples are however, found more stable to degradation than the uncapped samples. The stability of γ-Fe₂O₃ sample with large particle size (15.4 nm) is more than the sample with small particle size (10.2 nm). Fe₃O₄ having a particle size of 48 nm is however less stable than the smaller γ-Fe₂O₃ nanoparticles.     

Magnetic and calorimetric studies on rare-earth iron borates LnFe3(BO3)4 (Ln=Y, La-Nd, Sm-Ho)

A series of rare-earth iron borates having general formula LnFe₃(BO₃)₄ (Ln=Y, La-Nd, Sm-Ho) were prepared and their magnetic properties have been investigated by the magnetic susceptibility, specific heat, and ⁵⁷Fe Mössbauer spectrum measurements. These borates show antiferromagnetic transitions at low temperatures and their magnetic transition temperatures increase with decreasing Ln³⁺ ionic radius from 22 K for LaFe₃(BO₃)₄ to 40 K for TbFe₃(BO₃)₄. In addition, X-ray diffraction, specific heat, and differential thermal analysis (DTA) measurements indicate that the phase transition occurs for the LnFe₃(BO₃)₄ compounds with Ln=Eu-Ho, Y, and its transition temperature increases remarkably with decreasing Ln³⁺ ionic radius from 88 K for Ln=Eu to 445 K for Ln=Y.     

Controlled synthesis of single-crystalline Mg(OH)2 nanotubes and nanorods via a solvothermal process

The synthesis of Mg(OH)₂ one-dimensional (1D) nanostructures was systematically investigated in different solvents at various temperatures with Mg₁₀OH₁₈Cl₂·5H₂O nanowires as source materials. The results showed that the characters of the products, such as crystal size, shape, and structure, were strongly influenced by the solvent and temperature during the solvothermal process. 1D nanotubes of Mg(OH)₂, with 80-300 nm outer diameter, 30-80 nm wall thickness, and several tens of micrometers in length were obtained by choosing bidentate ligand solvents such as ethylenediamine and 1,6-diaminohexane as the reaction solvent. But when using monodentate ligand pyridine as the reaction solvent, the obtained samples showed nanorods morphology. The Mg(OH)₂ thus produced was analyzed by X-ray powder diffraction (XRD), transmission electron microscopy (TEM), high-resolution electron microscopy (HRTEM), and selected-area electron diffraction (SAED). The possible growth mechanism of the 1D nanostructure Mg(OH)₂ was discussed.     

Synthesis of Mn3O4 nanoparticles by thermal decomposition of a [bis(salicylidiminato)manganese(II)] complex

The present investigation reports on the novel synthesis of Mn₃O₄ nanoparticles using thermal decomposition and their physicochemical characterization. The Mn₃O₄ nanoparticle powder has been prepared using [bis(salicylidiminato)manganese(II)] as a precursor. The effect of oleyl amine and triphenylphosphine on the particle morphology has been investigated. Transmission electron microscopy (TEM) analysis demonstrated Mn₃O₄ nanoparticles with an average diameter of about 25 nm. The structural study by X-ray diffraction (XRD) indicates that these nanoparticles have a pure tetragonal phase. The phase pure samples were characterized using X-ray photoelectron spectroscopy (XPS) for both Mn 2p and Mn 3s levels. The values of binding energies are consistent with related values reported in the literature.