Synthesis of colloidal Mn2+:ZnO quantum dots and high-TC ferromagnetic nanocrystalline thin films

We report the synthesis of colloidal Mn(2+)-doped ZnO (Mn(2+):ZnO) quantum dots and the preparation of room-temperature ferromagnetic nanocrystalline thin films. Mn(2+):ZnO nanocrystals were prepared by a hydrolysis and condensation reaction in DMSO under atmospheric conditions. Synthesis was monitored by electronic absorption and electron paramagnetic resonance (EPR) spectroscopies. Zn(OAc)(2) was found to strongly inhibit oxidation of Mn(2+) by O(2), allowing the synthesis of Mn(2+):ZnO to be performed aerobically. Mn(2+) ions were removed from the surfaces of as-prepared nanocrystals using dodecylamine to yield high-quality internally doped Mn(2+):ZnO colloids of nearly spherical shape and uniform diameter (6.1 +/- 0.7 nm). Simulations of the highly resolved X- and Q-band nanocrystal EPR spectra, combined with quantitative analysis of magnetic susceptibilities, confirmed that the manganese is substitutionally incorporated into the ZnO nanocrystals as Mn(2+) with very homogeneous speciation, differing from bulk Mn(2+):ZnO only in the magnitude of D-strain. Robust ferromagnetism was observed in spin-coated thin films of the nanocrystals, with 300 K saturation moments as large as 1.35 micro(B)/Mn(2+) and T(C) > 350 K. A distinct ferromagnetic resonance signal was observed in the EPR spectra of the ferromagnetic films. The occurrence of ferromagnetism in Mn(2+):ZnO and its dependence on synthetic variables are discussed in the context of these and previous theoretical and experimental results.     

Synthesis of ZnO:Ga nanosized powders by the combustion method

The synthesis of ZnO:Ga(0.075 wt%) nanosized powders via combustion reaction at 145°C and subsequent calcination of the ground combustion product at 500–900°C was studied. Zinc and gallium nitrates were used as initial substances, and sucrose, as fuel. It was found that Ga₂O₃ nanoparticles are located on the ZnO particles and inhibit their growth.     

Synthesis and morphological characterization of nanocrystalline powders obtained by a gas condensation method

The preparation of nanocrystalline powders of Fe and Fe50Ni50 has been performed by a gas-condensation method under pure helium atmosphere. The characterization of the prepared materials which was carried out by means of Transmission Electron Microscopy, X-rays diffraction and Mössbauer Spectrometry, evidences for the presence of oxide phases. Fe and FeNi based ultrafine particles are observed with a size comprised within the range 10–70 nm and they occur as clusters or chains.     

Synthesis, structure and magnetic properties of nanocrystalline YMnO3

Nanocrystalline YMnO(3) has been prepared by wet chemical synthesis routes to obtain crystallites with sizes from 20 nm to bulk material. The crystal structure of hexagonal YMnO(3) nanocrystallites smaller than 80 nm deviates from bulk material in terms of unit cell distortion and unit cell volume. The ferrielectric displacements of Y(3+) cations along the polar c-axis decays progressively with decreasing size below 100 nm. Indications of weak ferromagnetism in the form of a narrow hysteresis loop and enhanced magnetic susceptibility below 43 K in 20 nm YMnO(3) nanoparticles is attributed to extrinsic effects. Low-temperature annealing of the 20 nm crystallites in an oxidizing atmosphere removed all traces of ferromagnetism, showing that this is not a size-induced property. Finally, formation of the competing metastable orthorhombic phase and the thermodynamically stable hexagonal phase is discussed with respect to oxidizing or reducing conditions during synthesis.     

Synthesis and magnetic properties of hexagonally packed ZnO nanorods

Large-scale uniform aligned ZnO nanorods with a hexagonal tip were successfully synthesized via a facile process at low temperature of (～140 °C) without using any additives and substrate. The process is based on a simple reaction of zinc powder and de-ionized water. The results reveal that the as-prepared ZnO products have an average length of 10 μm and a diameter in the range of 50–260 nm, possessing a single crystal wurtzite structure. The structure and morphology of the ZnO products are characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM) and energy dispersive X-ray spectrometer (EDX). The possible formation mechanism of nanorods is proposed in brief. The optical properties of grown products were characterized by room-temperature. The magnetic property was tested with a vibrating sample magnetometer at room temperature and revealed a high hysteresis loop indicating a strong ferromagnetic nature of as synthesized ZnO nanorods. The yield producing nanorods with this method includes ease, flexibility, fast being low cost and ineffective on environment free.     

Preparation and magnetic properties of RFeO<Subscript>3</Subscript> nanocrystalline powders

The rare-earth orthoferrites RFeO₃ (R, rare-earth element) crystallize in an orthorhombic distorted perovskite structure. RFeO₃ compounds exhibit interesting physical and chemical properties because of their ionic and electronic defects. Polycrystalline nano-sized RFeO₃ powders were synthesized by the sol–gel combustion method. X-ray powder diffraction indicated that nanocrystalline powders were single ReFeO3 phase, which are agglomerated with average crystallite size of 60–90 nm estimated with the Scherrer’s equation. Magnetic measurements were carried out using a superconducting quantum interference device magnetometer. The influence on hysteresis curve of electronic structure of rare-earth element was investigated for R = Y, La and Nd. Varied magnetic behaviors were observed in these compounds, which are believed to be associated with the different interactions of Fe and rare earths.     

Biocidal activity of nanocrystalline silver powders and particles

While the activity of the SMAD powders is lower than that of pure silver nitrate, it has the ability to kill bacteria very effectively and over long periods of time.     

SrZrO3 powders obtained by chemical method: Synthesis,characterization and optical absorption behaviour

Strontium zirconate (SrZrO₃) powders have been synthesized by the polymeric precursor method after heat treatment at different temperatures for 2 h in oxygen atmosphere. The decomposition of precursor powder was followed by thermogravimetric analysis, X-ray diffraction (XRD) and Fourier transform Raman (FT-Raman). The UV–vis absorption spectroscopy measurements suggested the presence of intermediary energy levels in the band gap of structurally disordered powders. XRD, Rietveld refinement and FT-Raman revealed that the powders are free of secondary phases and crystallizes in the orthorhombic structure.     

Ceramic materials made of CdTe and Cd-Zn-Te nanocrystalline powders

In the present study newly produced semiconductor ceramic nanopowder materials made of CdTe and Cd_1−xZn_xTe (CZT) are considered. Common features and differences in microstructures, phase transformations, grain growth and properties of the ceramic materials of the binary and ternary compositions are studied.      

球形纳米氧化锌的合成

本文报道了一种使用流变相法制备球形纳米氧化锌的方法.首先将氧化锌和尿素按摩尔比1:4混合均匀,加适量水调制成流变态,在300℃反应生成胶状物;然后将胶状物在高速搅拌下水解,将水解产物在120℃下分解;最后研究了热分解产物的表面形貌与粒度分布.实验结果表明在120℃左右生成白色球形纳米ZnO粉体,粒度分布在30-80nm...     

Synthesis, structure and magnetic behaviour of mixed metal leucophosphite

A synthetic analogue of leucophosphite, an iron phosphate, was synthesized hydrothermally at 180 °C and its chemical composition determined to be {K[(FeV)(PO₄)₂(OH)(H₂O)]·H₂O}. The compound crystallizes in the monoclinic P2₁/c space group, with a=9.7210(19) Å, b=9.6500(19) Å, c=12.198(4) Å and β=128.569(18)°. While the original all-iron compound is reported to be antiferromagnetic, the inclusion of substitutional vanadium(III) ions renders the structure ferrimagnetic. Diffraction studies and magnetic characterization show that iron and vanadium are disordered throughout the crystallographic sites. The magnetic behaviour of this system was interpreted in terms of a classic ferrimagnetic mean field model, consisting of two antiferromagnetically coupled non-crystallographic “sublattices”.     

Preparation and characterization of Al and Mn doped ZnO (ZnO: (Al,Mn)) transparent conducting oxide films

This paper presents the electro-optical, chemical and structural properties of doped-ZnO films deposited by DC-reactive magnetron sputtering at room temperature using the bi-dopant Al and Mn. A minimum resistivity of 3.46×10⁻⁴ Ω cm, exceeding 75.0% average transmittance (380–800 nm), and fundamental band gap of 3.48±0.01 eV have been obtained. XPS analyses show that Zn uniformly remains in the valence state of Zn²⁺; all of the Al and a little amount of Mn with valence state of Mn⁴⁺ are supposed to have donor effect, while dominant Mn²⁺ will induce to form more oxygen vacancies and this proposal has been verified by O 1s XPS results. It has been concluded that the presence of more oxygen vacancies will attenuate the effect of hybridization of p–d orbitals in the matrix of ZnO. It has been found that all the as-deposited films have c-axis preferred orientation with flat and smooth surface (RMS surface roughness is of the order of ∼3 nm over 5×5 μm² area).     

Synthesis and properties of magnetic semiconductor InSb〈Mn,Cd〉

Polycrystalline indium antimonide samples codoped with manganese (0.8–1 at %) and cadmium (3.9 at %) are prepared by quenching from melt. Despite the high contents of these dopants, only InSb maxima are observed in X-ray diffraction patterns of these samples. As probed by magnetic studies, the samples are ferrimagnets having Curie points of about 577 K and room-temperature specific magnetizations of σ ≈ 0.5 G cm³/g (H = 6 kOe). We suggest that the magnetic properties of the samples are dictated by InSb〈Mn,Cd〉 microinclusions, which are located in grain boundaries and dislocations.     

Preparation of magnetic nanocrystalline Mn0.5Mg0.5Fe2O4 and kinetics of thermal decomposition of precursor

The spinel Mn_0.5Mg_0.5Fe₂O₄ was obtained via calcining Mn_0.5Mg_0.5Fe₂(C₂O₄)₃·5H₂O above 400 °C in air. The precursor and its calcined products were characterized by thermogravimetry and differential scanning calorimetry, Fourier transform FT-IR, X-ray powder diffraction, scanning electron microscopy, energy dispersive X-ray spectrometer, and vibrating sample magnetometer. The results showed that Mn_0.5Mg_0.5Fe₂O₄ obtained at 600 °C had a specific saturation magnetization of 46.2 emu g^–1. The thermal decomposition of Mn_0.5Mg_0.5Fe₂(C₂O₄)₃·5H₂O below 450 °C experienced two steps which involved, at first, the dehydration of five water molecules and then decomposition of Mn_0.5Mg_0.5Fe₂(C₂O₄)₃ into spinel Mn_0.5Mg_0.5Fe₂O₄ in air. Based on Starink equation, the values of the activation energies associated with the thermal decomposition of Mn_0.5Mg_0.5Fe₂(C₂O₄)₃·5H₂O were determined.     

p-Type behaviour of electrodeposited ZnO:Cu films

Cu-doped ZnO (ZnO:Cu) thin films and ZnO/ZnO:Cu homojunction devices were electrodeposited on conductive glass substrates in a non-aqueous electrolyte containing Cu and Zn salts. The Cu content of the films is proportional to the Cu/Zn precursor ratio in the deposition electrolyte. ZnO:Cu was found to be of a hexagonal wurtzite structure with (002) preferred orientation. A transition from n-type to p-type was observed for ZnO:Cu films with a Cu/Zn ratio higher than 2% as inferred from the change in the direction of the photocurrent. The rectifying characteristics shown by homojunction devices further confirm the p-type conductivity of ZnO:Cu layers.     

Thermal behaviour of mechanochemically synthesized nanocrystalline CuS

Thermal behaviour of mechanochemically synthesized nanocrystalline CuS particles by high-energy milling in an industrial mill has been studied. Structure properties were characterized by X-ray powder diffraction that reveals the formation of copper sulphide CuS as well as of copper sulphate CuSO₄·5H₂O. Thermal properties of the as-prepared products were studied by the differential scanning calorimetry together with X-ray inspection for detection by pass products formed. The decomposition of the as-prepared sample has been studied too. Thermal stability of the anhydrous CuSO₄ formed by the thermal decomposition is lower than the thermal stability of non-milled samples. The final product of the thermal decomposition is metallic copper instead of Cu₂O, which is stable up to 1100 °C. Differential scanning calorimetry (DSC) analysis proved that the percentage of chalcantite in the covellite mechanochemically synthesized by high-energy milling is 48-51%.     

Characteristics and sintering behaviour of zirconia ultrafine powders

Coprecipitation from water solution of chlorides was used to obtain yttria-stabilized zirconia powders. It was shown that precalcination processing of the coprecipitated gel greatly affects the microstructure of the resultant powder as well as its cold compaction behaviour and hence its sinterability. Relative densities of +98% theoretical have been achieved at sintering temperature as low as 1300°C.     

Preparation and characterization of nanocrystalline ZnO by direct precipitation method

Nanocrystalline ZnO was prepared with ZnCl₂·2H₂O and (NH₄)₂CO₃ as raw materials by direct precipitation method. The precursor was proved to be [Zn₅(OH)₆(CO₃)₂] by TG-DTG-DTA and IR analysis. This precursor was calcined at 300°C for 1, 2 and 3 hours respectively, and then the nanocrystalline ZnO of different grain size were obtained. The nanocrystalline ZnO was characterized using X-ray diffraction (XRD), TEM and Brunner-Emmett-Teller method (BET). Experimental results for nanocrystalline ZnO showed that the minimum size was about 8nm, the maximum was about 15 nm and the mean grain size was 12 nm, the surface area was 80.56 m²/g and the purity was 99.9% when the precursor was calcined at 300°C for 2 h. __________ Translated from Journal of Inner Mongolia Normal University (Natural Science Edition), 2006, 35(1) (in Chinese)     

Pure and Gd-based Li,Na, Mn or Fe codoped ZnO nanoparticles: Insights into the magnetic and photocatalytic properties

The ferromagnetic and photocatalytic properties of pure ZnO, Zn_0.97Gd_0.01Li_0.02O, Zn_0.97Gd_0.01Na_0.02O, Zn_0.97Gd_0.01Mn_0.02O and Zn_0.97Gd_0.01Fe_0.02O nanoparticles prepared by sol-gel technique were investigated. The XRD, EDX, HR-TEM, FTIR and diffuse reflectance analyses confirm the formation of single phase ZnO wurtzite structure with effective incorporation of Gd/Li, Na, Mn or Fe ions into ZnO host lattice. Based on Kubelka-Munk equation, the optical band gap of pure ZnO nanoparticles was estimated to be 3.22 eV and implantation of Gd-based dual dopants induces red shifts between 0.01 and 0.29 eV. For pure ZnO nanoparticles, noticeable ferromagnetic performance was observed with saturation magnetization of 0.0133 emu/g and coercivity of 85 Oe. The binary dopants of Gd/Mn or Na induce strong enhancements in the saturation magnetization of pure ZnO nanoparticles. Where, Zn_0.97Gd_0.01Na_0.02O and Zn_0.97Gd_0.01Mn_0.02O samples exhibited perfect hysteresis loops with saturation magnetization of 0.34 and 0.717 emu/g, respectively. Higher photocatalytic activity, 97%, for methyl orange degradation was observed for Zn_0.97Gd_0.01Na_0.02O nanoparticles within 210 min under UV irradiation. The particles size and agglomeration, ionic radii of dopants and recombination centers have main effects on the photocatalytic activity performance of ZnO nanoparticles. The dual dopants of Gd/Mn efficiently trigger the room temperature ferromagnetism of the pure ZnO; but Gd/Na blend revealed the best effect in methyl orange degradation (97%).