Photopyroelectric spectroscopy of Sb<Subscript>2</Subscript>O<Subscript>3</Subscript> - ZnO ceramics

Photopyroelectric spectroscopy is used to study the band-gap energy of the ceramic (ZnO + xSb₂O₃), x = 0.1 - 1.5 mol% and the ceramic (ZnO + 0.4 mol%  Bi₂O₃ + xSb₂O₃), x = 0 - 1.5 mol% sintered at isothermal temperature, 1280 °C, for 1 and 2 hours. The wavelength of incident light, modulated at 9 Hz, is kept in the visible range and the photopyroelectric spectrum with reference to doping level is discussed. The band-gap energy is reduced from 3.2 eV, for pure ZnO, to 2.86, 2.83 eV for the samples without Bi₂O₃at 0.1 mol% of Sb₂O₃ for 1 and 2 hours of sintering time, respectively. It is reduced to 2.83, 2.80 eV for the samples with Bi₂O₃ at 0 mol% of Sb₂O₃ for 1 and 2 hours of sintering time, respectively. The steepness factor σ_A which characterizes the slop of exponential optical absorption is discussed with reference to the doping level. The phase constitution is determined by XRD analysis; microstructure and compositional analysis of the selected areas are analyzed using SEM and EDX.     

One-step synthesis of colloidal Mn<Subscript>3</Subscript>O<Subscript>4</Subscript> and γ-Fe<Subscript>2</Subscript>O<Subscript>3</Subscript> nanoparticles at room temperature

A facile room-temperature synthesis has been developed to prepare colloidal Mn₃O₄ and γ-Fe₂O₃ nanoparticles (5 to 25 nm) by an ultrasonic-assisted method in the absence of any additional nucleation and surfactant. The morphology of the as-prepared samples was observed by transmission electron microscopy. High-resolution transmission electron microscopy observations revealed that the as-synthesized nanoparticles were single crystals. The magnetic properties of the samples were investigated with a superconducting quantum interference device magnetometer. The possible formation process has been proposed.     

Controlled synthesis of photoluminescent Bi<Subscript>4</Subscript>Ti<Subscript>3</Subscript>O<Subscript>12</Subscript> nanoparticles from metal-organic polymeric precursor

Bi₄Ti₃O₁₂ (BIT) nanoparticles with a narrow average particle size distribution in the range of 11–46 nm was synthesized via a metal-organic polymeric precursor process. The crystallite size and lattice parameter of BIT were determined by XRD analysis. At annealing temperatures >550 °C, the orthorhombic BIT compound with lattice parameters a = 5.4489 Å, b = 5.4147 Å, and c = 32.8362 Å was formed while at lower annealing temperatures orthorhombicity was absent. Reaction proceeded via the formation of an intermediate phase at 500 °C with a stoichiometry close to Bi₂Ti₂O₇. The particle size and the agglomerates of the primary particles have been confirmed by FESEM and TEM. The decomposition of the polymeric gel was ascertained in order to evaluate the crystallization process from TG-DSC analysis. Raman spectroscopy was used to investigate the lattice dynamics in BIT nanoparticles. In addition, investigation of the dependence of the visible emission band around the blue–green color emission on annealing temperatures and grain sizes showed that the effect of grain size plays important roles, and that oxygen vacancies may act as the radiative centers responsible for the observed visible emission band.     

Up-conversion emissions of Er<Superscript>3+</Superscript>-Yb<Superscript>3+</Superscript> codoped Al<Subscript>2</Subscript>O<Subscript>3</Subscript> nanoparticles by the arc discharge synthesis method

The Er³⁺-Yb³⁺ codoped Al₂O₃ nanoparticles with an average particle size of about 50 nm have been synthesized by an arc discharge synthesis method. The green and red up-conversion emissions centered at about 526, 547 and 677 nm, corresponding respectively to the ²H_11/2→⁴I_15/2, ⁴S_3/2→⁴I_15/2 and ⁴F_9/2→⁴I_15/2 transitions of Er³⁺, were detected by a 978-nm semiconductor laser diode excitation. The Annealing has evident effect on the up-conversion emissions of the samples: The red up-conversion emission is noticeable before annealing; however, the green up-conversion emission becomes predominant after annealing. The mixture of (Er,Yb)₃Al₅O₁₂ and α-(Al,Er,Yb)₂O₃ phases is more favorable for green up-conversion emissions due to an enhancement of the ESA (I) of ⁴I_11/2+a photon→⁴F_7/2 and ET (III) of ²F_5/2(Yb³⁺)+⁴I_11/2(Er³⁺)→²F_7/2(Yb³⁺)+⁴F_7/2(Er³⁺) processes. The two-photon absorption up-conversion process is involved in the green and red up-conversion emissions. The results have proved that arc discharge synthesis is a new promising preparation technology for optical materials. Supported by National Natural Science Foundation of China (Grant No. 10804015), the Scientific Research Foundation for Doctor of Liaoning Province (Grant No. 20071095), and the Educational Committee Foundation of Liaoning Province (Grant No. 2008123)     

Plasmachemical synthesis and basic properties of CoFe<Subscript>2</Subscript>O<Subscript>4</Subscript> magnetic nanoparticles

Cobalt-ferrite (CoFe₂O₄) nanoparticles (CFNPs) are obtained using direct plasmachemical synthesis in the plasma of a low-pressure arc discharge. The formation of the CFNPs with an average size of 9 nm and a narrow granulometric composition is established employing the methods of X-ray structure analysis and transmission microscopy. The CFNP behavior upon high-temperature annealing is analyzed. The CFNP functional groups are determined using the infrared Fourier spectrum. The results of the X-ray energy dispersion confirm the correspondence of the ratio of the number of atoms of each material to the nominal stoichiometry. The basic magnetic properties of the obtained and annealed samples are investigated at room temperature using the vibrating spectrum magnetometry (VSM).     

Room temperature synthesis of single-crystal Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> nanoparticles with superparamagnetic property

Single-crystal Fe₃O₄ nanoparticles with uniform size and relatively better monodispersity have been successfully synthesized via a facile room temperature coprecipitation route in the present of poly(vinyl pyrrolidone) (PVP). This method does not require high temperature, expensive and toxic starting materials, complicated procedure and toxic organic solvents. The magnetic properties of as-prepared samples were recorded on a superconducting quantum interference device magnetometer. Its blocking temperature is 140 K. The hysteresis loops of single-crystal Fe₃O₄ nanoparticles at 300 K and 10 K show the transition from superparamagnetic to ferromagnetic behavior. And the maintenance of high saturation magnetization ascribes to the single-crystalline nature of these Fe₃O₄ nanoparticles. PACS 75.50.K; 75.70.C     

Temperature-controlled synthesis of Ga<Subscript>2</Subscript>O<Subscript>3</Subscript> nanobelts and nanosheets

We have investigated the effect of growth temperature on structural morphology and photoluminescence (PL) properties of as-synthesized gallium oxide (Ga₂O₃) nanostructures. The products consisted of Ga₂O₃ nanobelts and nanosheets (i.e. wider nanobelts), which had monoclinic crystalline structures. The average width of structures grown at 1000 °C was relatively greater than those at 800 °C, revealing that higher temperature favored the formation of nanosheets. PL measurements of 800 °C- and 1000 °C-grown samples indicated that both samples exhibited a broad emission band peaked around the blue-light region, while only the 800 °C-grown sample showed a red peak. PACS 81.07.-b; 81.05.Je; 61.10.Nz; 68.37.Hk; 68.37.Lp     

Gas sensor based on nanosize In<Subscript>2</Subscript>O<Subscript>3</Subscript>:Ga<Subscript>2</Subscript>O<Subscript>3</Subscript> film

Nanosize films of In₂O₃:Ga₂O₃ (96:4 weight %) have been deposited on a glassceramic substrate by the method of rf magnetron sputtering. The surfaces of fabricated films were studied with use of a scanning electron microscope; sizes of grains were determined and the thicknesses of films were measured. In order to prepare a gas-sensitive structure, a thin catalytic palladium layer and ohmic comb contacts were deposited on the In₂O₃:Ga₂O₃ film surface by the method of ion-plasma sputtering. The sensitivity of sensors based on the glassceramic/In₂O₃:Ga₂O₃ (96:4 weight %)/Pd structure to different concentrations of propane and butane gas mixture, as well as to methane was investigated at temperatures of working substance from 250 to 300°C.     

Synthesis and characterization of hollow nanoparticles of crystalline Gd<Subscript>2</Subscript>O<Subscript>3</Subscript>

Although Gd₂O₃ (gadolinia) nanoparticle is the subject of intense research interest due to its magnetic property as well as controllable emission wavelengths by doping of various lanthanide ions, it is known to be difficult to prepare monodisperse crystalline gadolinia nanoparticles because it requires high temperature thermal annealing process to enhance the crystallinity. In this article, we demonstrate the synthesis of hollow nanoparticles of crystalline Gd₂O₃ by employing poly(N-vinylpyrrolidone) (PVP) to stabilize the surface of Gd(OH)CO₃·H₂O nanoparticles and to successively form SiO₂ shell as a protecting layer to prevent aggregation during calcinations processes. Silica shells could be selectively removed after calcinations by a treatment with basic solution to give hollow nanoparticles of crystalline Gd₂O₃. The formation mechanism of hollow nanoparticles could be suggested based on several characterization results of the size and shape, and crystallinity of Gd₂O₃ nanoparticles by TEM, SEM, and XRD.     

Hydrothermal synthesis and magnetic properties of CuSb<Subscript>2</Subscript>O<Subscript>6</Subscript> nanoparticles and nanorods

Nanoparticles and nanorods of CuSb₂O₆ are prepared by hydrothermal method and its high temperature α-phase is stabilized at room temperature. The average size of the nanoparticles is ca. 13.7 nm. The nanorods, with a width of ca. 20 nm and an aspect ratio of ca. 5, are the agglomerates composing of smaller nanoparticles with an average size of ca. 8.3 nm. Compared with the high temperature α-phase of bulk sample at 400 K, the lattice of nanophases elongated in ab plane and compressed along c direction. The CuSb₂O₆ nanoparticles exhibit predominant paramagnetic phenomenon. The difference in magnetic properties of the nanoparticles and nanorods indicates the interfacial interaction of agglomerated nanoparticles.     

Thermal sensors based on Sb<Subscript>2</Subscript>Te<Subscript>3</Subscript> and (Sb<Subscript>2</Subscript>Te<Subscript>3</Subscript>)<Subscript>70</Subscript>(Bi<Subscript>2</Subscript>Te<Subscript>3</Subscript>)<Subscript>30</Subscript> thin films

Thin films of Sb₂Te₃ and (Sb₂Te₃)₇₀(Bi₂Te₃)₃₀ alloy and have been deposited on precleaned glass substrate by thermal evaporation technique in a vacuum of 2?×?10^?6 Torr. The structural study was carried out by X-ray diffractometer, which shows that the films are polycrystalline in nature. The grain size, microstrain and dislocation density were determined. The Seebeck coefficient was determined as the ratio of the potential difference across the films to the temperature difference. The power factor for the (Sb₂Te₃)₇₀ (Bi₂Te₃)₃₀ and (Sb₂Te₃) is found to be 19.602 and 1.066 of the film of thickness 1,500 Å, respectively. The Van der-Pauw technique was used to measure the Hall coefficient at room temperature. The carrier concentration was calculated and the results were discussed.     

Synthesis of CoFe<Subscript>2</Subscript>O<Subscript>4</Subscript> nanoparticles with tunable magnetism by the modified hydrothermal method

Cobalt ferrite (CoFe₂O₄) nanoparticles were synthesized by using the hydrothermal route with the addition of trisodium citrate dihydrate (Na₃CA·2H₂O). The formation of CoFe₂O₄ nanoparticles with size ranging from 13 to 19 nm was confirmed by X-ray diffraction, energy dispersive X-ray analysis, and Fourier transform infrared spectroscopy; the clear-cut sharp of the nanoparticles was observed by transmission electron microscopy. By these characterization methods, the evolution of lattice constant and morphologies of the nanoparticles with the addition of Na₃CA·2H₂O is observed. Furthermore, the magnetic hysteresis loops measured at room temperature indicate that the magnetic properties of the products also show clear relationship with the masses of Na₃CA·2H₂O. For example, coercivity and high-field paramagnetic susceptibility increase with the increasing masses of Na₃CA·2H₂O, whereas the saturation magnetization and the effective magnetic anisotropy constant have the maximum values as the mass of Na₃CA·2H₂O is 1 g. This change of magnetic properties is related with the expanded lattice and the varied size and shape because of the addition of Na₃CA·2H₂O.     

Synthesis of In<Subscript>2</Subscript>O<Subscript>3</Subscript>nanoparticles by thermal decomposition of a citrate gel precursor

This paper describes the synthesis of indium oxide by a modified sol–gel method, and the study of thermal decomposition of the metal complex in air. The characterization of the intermediate as well as the final compounds was carried out by thermogravimetry, differential thermal analysis, Fourier transform infrared spectroscopy, X-ray diffraction, transmission electron microscopy, and small angle X-ray scattering. The results show that the indium complex decomposes to In₂O₃ with the formation of an intermediate compound. Nanoparticles of cubic In₂O₃ with crystallite sizes in the nanosize range were formed after calcination at temperatures up to 900°C. Calcined materials are characterized by a polydisperse distribution of spherical particles with sharp and smooth surfaces.This revised version was published online in August 2005 with a corrected issue number.     

Interaction of carbon monoxide with In<Subscript>2</Subscript>O<Subscript>3</Subscript> and In<Subscript>2</Subscript>O<Subscript>3</Subscript>-Au nanocomposite

This is an IR spectroscopic study of the interaction of CO with In₂O₃ and the nanocomposite In₂O₃-Au. A mechanism for low-temperature detection of CO on nanocomposite In₂O₃-Au can be determined from these data. This process includes catalytic oxidation of CO through formation of intermediate complexes involving hydroxyl groups of In₂O₃.     

Spectral-luminescent investigations of glasses and glass-ceramic materials in Bi<Subscript>2</Subscript>O<Subscript>3</Subscript>-GeO<Subscript>2</Subscript>-Fe<Subscript>2</Subscript>O<Subscript>3</Subscript> system

Glasses of 2Bi₂O₃-3GeO₂-xFe₂O₃ composition, where x = 0–1.5, are obtained under oxidizing and reducing conditions. Glass-ceramic materials are produced by the thermal treatment of the glasses, the properties of which, as well as those of the original glasses, are studied by the methods of X-ray phase analysis and optical and luminescent spectroscopy. It is found that the Fe³⁺/Fe²⁺ ion ratio in the samples changes depending on the synthesis conditions of the original glasses and crystallization process.     

Conductivity and spectroscopic studies of Li<Subscript>2</Subscript>O-V<Subscript>2</Subscript>O<Subscript>5</Subscript>-B<Subscript>2</Subscript>O<Subscript>3</Subscript> glasses

Lithium vanadium-borate glasses with the composition of 0.3Li₂O–(0.7-x)B₂O₃–xV₂O₅ (x?=?0.3, 0.325, 0.35, 0.375, 0.4, 0.425, 0.45, and 0.475) were prepared by melt-quenching method. According to differential scanning calorimetry data, vanadium oxide acts as both glass former and glass modifier, since the thermal stability of glasses decreases with an increase in V₂O₅ concentration. Fourier transform infrared spectroscopy data show that the vibrations of [VO₄] structural units occur at V₂O₅ concentration of 45 mol%. It is established that the concentration of V⁴⁺ ions increases exponentially with the growth of vanadium oxide concentration. Direct and alternative current measurements are carried out to estimate the contribution both electronic and ionic conductivities to the value of total conductivity. It is shown that the electronic conductivity is predominant in the total one. The glass having the composition of 0.3Li₂O-0.275B₂O₃-0.475V₂O₅ shows the highest electrical conductivity that has the value of 7.4?×?10^?5 S cm^?1 at room temperature.     

Photoluminescence of nanoparticles of (Ga<Subscript>2</Subscript>S<Subscript>3</Subscript>)<Subscript>0.95</Subscript>(Eu<Subscript>2</Subscript>O<Subscript>3</Subscript>)<Subscript>0.05</Subscript> solid solution

We have ground bulk samples to obtain nanoparticles of (Ga₂S₃)_1–x (Eu₂O₃) _x solid solutions, the sizes of which were determined using an atomic force microscope. The photoluminescence spectra of the nanoparticles were studied in the temperature interval 77–300 K. We have established the mechanisms for emission and transfer of energy from the matrix to the rare-earth ion, and we determined the Stokes shift (ΔS = 0.7 eV), the Huang–Rhys parameter (S = 16), and the optical phonon energy (ħ−ω = 23 meV).     

Nano-MnFe<Subscript>2</Subscript>O<Subscript>4</Subscript> powder synthesis by detonation of emulsion explosive

Nano-MnFe₂O₄ powders were synthesized by detonation of specially prepared emulsion explosives. X-ray diffraction and transmission electron microscopy were carried out to characterize the as-prepared powders. The results indicated that relatively finely dispersed spherical powders were obtained when the content of RDX in the emulsion explosives was 9.18 wt. %. A certain content of internal-phase ammonium nitrate was not only favorable to control the ingredients of the detonation products, but also advantageous to stabilize the detonation structure of the emulsion explosive according to differential thermogravimetry experimental results. PACS 81.07.Bc; 81.20.-n     

Characteristic features of optical absorption for Gd<Subscript>2</Subscript>O<Subscript>3</Subscript> and NiO nanoparticles

The technical approach to determination of the structural and optical parameters of oxides with reduced dimensionality based on optical absorption measurements is described by example of gadolinium and nickel oxides. It was established that the temperature behavior of fundamental absorption edge for oxide nanoparticles is similar with the bulk materials with crystal structure. At the same time, the energy characteristics (band gap and effective phonon energies) for low-dimensional oxides are found to be significantly different from their bulk counterparts. The presented methodological method to obtain of qualitative and quantitative correlations of structural and optical characteristics provides novel reliable knowledge of nanoscaled 3d and 4f–metal oxide materials that is useful for development of their practical applications.