Electrical and gas sensing properties of self-aligned copper-doped zinc oxide nanoparticles

Electrical and gas sensing properties of nanocrystalline ZnO:Cu, having Cu X wt% (X = 0.0, 0.5, 1.0, and 1.5) in ZnO, in the form of pellet were investigated. Copper chloride and zinc acetate were used as precursors along with oxalic acid as a precipitating reagent in methanol. Material characterization was done by X-ray diffraction (XRD), scanning electron microscopy (SEM), field emission scanning electron microscopy (FE-SEM) and inductive coupled plasma with optical emission spectrometry (ICP-OES). FE-SEM showed the self-aligned Cu-doped ZnO nano-clusters with particles in the range of 40-45 nm. The doping of 0.5% of copper changes the electrical conductivity by an order of magnitude whereas the temperature coefficient of resistance (TCR) reduces with increase in copper wt% in ZnO. The material has shown an excellent sensitivity for the H₂, LPG and CO gases with limited temperature selectivity through the optimized operating temperature of 130, 190 and 220 °C for H₂, LPG and CO gases, respectively at 625 ppm gas concentration. The %SF was observed to be 1460 for H₂ at 1% Cu doping whereas the 0.5% Cu doping offered %SF of 950 and 520 for CO and LPG, respectively. The response and recovery time was found to be 6 to 8 s and 16 s, respectively.     

Influence of structural ordering on electrical conductivity of nanostructured manganese zinc ferrite

In the present study, nanostructured manganese zinc ferrite of 11 nm grain size was synthesized by co-precipitation technique and subsequently suitably heat treated to obtain higher grain sizes. The plot of temperature dependence of dc conductivity shows the semiconducting nature of samples. The observed changes in the electrical conductivity have been attributed with the influence of structural ordering upon annealing. The observed decrease in conductivity when the grain size is increased from 11 to 69 nm upon annealing is clearly due to the structural ordering which is evident from FESEM.     

Nanostructured zinc oxide films synthesized by successive chemical solution deposition for gas sensor applications

Nanostructured ZnO thin films have been deposited using a successive chemical solution deposition method. The structural, morphological, electrical and sensing properties of the films were studied for different concentrations of Al-dopant and were analyzed as a function of rapid photothermal processing temperatures. The films were investigated by X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy, X-ray photoelectron and micro-Raman spectroscopy. Electrical and gas sensitivity measurements were conducted as well. The average grain size is 240 and 224 Å for undoped ZnO and Al-doped ZnO films, respectively. We demonstrate that rapid photothermal processing is an efficient method for improving the quality of nanostructured ZnO films. Nanostructured ZnO films doped with Al showed a higher sensitivity to carbon dioxide than undoped ZnO films. The correlations between material compositions, microstructures of the films and the properties of the gas sensors are discussed.     

Microwave-assisted hydrothermal synthesis of coralloid nanostructured nickel hydroxide hydrate and thermal conversion to nickel oxide

Coralloid nanostructured nickel hydroxide hydrate has been successfully synthesized by a simple microwave-assisted hydrothermal process using nickel sulfate hexahydrate as precursor and urea as hydrolysis-controlling agent. A pure coralloid nanostructured nickel oxide can be obtained from the nickel hydroxide hydrate after calcination at 400 °C. The thermal property, structure and morphology of samples were characterized by thermogravimetry (TG), temperature-programmed reduction (TPR), X-ray (XRD), infrared spectroscopy (IR), scanning electron microscopy (SEM) and transmission electron microscopy (TEM).     

Synthesis of flower- and rod-like nickel sulfide nanostructures by an organic-free hydrothermal process

Well-crystalline flower- and rod-like NiS nanostructures have been synthesized by an organic-free hydrothermal process at a low temperature of 200 °C. X-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM) were employed to characterize the as-synthesized NiS nanostructures. The effects of temperature and reaction time on the morphology have been also investigated. The two-step flake-cracking mechanism for the formation of flower- and rod-like NiS nanostructures was discussed. The products were also investigated by photoluminescence (PL) spectroscopy.     

Submicrometer-sized hollow nickel spheres synthesized by autocatalytic reduction

A facile method to fabricate submicrometer-sized hollow nickel spheres by autocatalyzing the redox reaction around a sacrificial colloidal particle surface is presented in this paper. The size distribution of these spheres can be controlled by regulating the concentration of the alkali solution. The hollow nickel particles were characterized by field emission scanning electron microscopy, transmission electron microscopy and X-ray powder diffraction. The hollow spheres produced by this process may have potential applications in many fields, including chemistry, biotechnology and materials science.     

Size-dependent blue luminescent CdS nanocrystals synthesized through a single-source molecular precursor route

In this paper, we report on the synthesis of size-dependent blue luminescent CdS nanocrystals by using a new nonhydrolytic single-source molecular method. The size of the synthesized CdS nanocrystals could be easily controlled by adjusting the ratio of reaction sources under inert atmosphere. The studies on the optical properties reveal an obvious size-dependent photoluminescence characteristic of the synthesized nanocrystals.     

Synthesis and characterization of nickel ferrite magnetic nanoparticles

Nickel ferrite (NiFe₂O₄) nanoparticles are prepared by a polyvinyl alcohol (PVA) assisted sol-gel auto-combustion method. The structure, composition, morphology and magnetic properties of the gel precursor are characterized by powder XRD, FT-IR, TGA, HR-SEM, TEM, HR-TEM and VSM. XRD confirms the formation of single-phase nickel ferrite with space group of Fd3m and inverse spinel structure. The vibration properties of nanoparticles are analysed by FT-IR spectrum. The thermal decomposition of the gel precursors is investigated by TGA. HR-SEM and TEM images show that the particles have spherical shape with particle size in the range of ∼30 nm and consistent with XRD result. The magnetic properties of these nanoparticles are studied for confirming the ferromagnetic behaviour at room temperature.     

Synthesis and characterization of porous ZnO nanoparticles by hydrothermal treatment of as pure aqueous precursor

The presence of the complexing agents in the growth solution poses risk of the unintentional doping in the synthesized product and hence is likely to adversely affect the intrinsic properties. Herein we report the synthesis of ZnO nanoparticles with porous microstructure using pure aqueous precursor. Crystalline ZnO nanoparticles were synthesized by thermal treatment of aqueous solution of zinc acetate in an open bath. The size of the nanocrystals was controlled by changing the initial precursor concentration. The structural and optical properties of the synthesized nanocrystals were analyzed by X-ray diffraction, high resolution transmission electron microscopy, UV-vis absorption and room temperature photoluminescence measurement techniques. The TEM and UV-vis spectral signature analyses confirmed the formation of dispersed single crystalline ZnO nanoparticles. The nanopowders were found to have disordered mesoporous structure. The synthesized nanocrystals exhibited characteristic band edge emission as well as to surface defect related deep level visible luminescence.     

Effect of finite size on the magnetization behavior of nanostructured nickel oxide

Nanostructured nickel oxide samples having different average particle sizes are synthesized through a wet chemical route. Room temperature magnetic hysteresis of the samples are recorded using a vibrating sample magnetometer. The magnetic properties of the samples are found to be markedly different from those of single crystalline nickel oxide. The sample with an average particle size of 2-3 nm showed superparamagnetism with magnetization curves defined by the Langevin function. Anomalously large uncompensated magnetic moment associated with this sample is attributed to the multisublattice magnetic structure. Interestingly, samples with larger average particle sizes of 13 and 18 nm exhibited superantiferromagnetism with the magnetization curves varying linearly with applied field and susceptibility values larger than that of bulk nickel oxide. The results highlight the importance of surface atoms and surface driven spin rearrangements in determining the magnetic properties of nanostructured nickel oxide.     

CuBi2O4 single crystal nanorods prepared by hydrothermal method: Growth mechanism and optical properties

The synthesis of copper bismuth oxide (CuBi₂O₄) nanorods with single crystal structure by hydrothermal method is first reported here. The prepared CuBi₂O₄ nanorods are characterized by X-ray diffractometer, scanning electron microscopy, transmission electron microscopy (TEM) and high resolution TEM. It is found that the concentration of reagent cupric acetate has strong effect on the purity and microstructure of the prepared samples. The growth process is investigated in detail. It is proposed that the nanorods are evolved from spherical particles with oriented attachment mechanism followed by dissolution-splitting process. The optical properties of the samples are detected by UV-vis spectrometer and photoluminescence spectrometer and exhibit strong dependence on surface defect states and microstructure feature, which is mainly determined by preparation conditions.     

Synthesis and electrochemical behavior of nanostructured cauliflower-shape Co-Ni/Co-Ni oxides composites

Nanostructured Co-Ni/Co-Ni oxides were electrochemically deposited onto stainless steel electrode by electrochemical method and characterized for their structural and supercapacitive properties. The SEM images indicated that the obtained Co-Ni/Co-Ni oxides had cauliflower-type nanostructure. The X-ray diffraction pattern showed the formation of Co₃O₄, NiO, Co and Ni. The EDX elemental mapping images indicated that Ni, Co and O are distributed uniformly. The deposited Co-Ni/Co-Ni oxides showed good supercapacitive characteristics with a specific capacitance of 331 F/g at 1 mA/cm² current density in 1 M KOH electrolyte. A mechanism of the formation of cauliflower-shape Co-Ni/Co-Ni oxides was proposed. A variety of promising applications in the fields such as energy storage devices and sensors can be envisioned from Co-Ni/Co-Ni oxides.     

Microwave hydrothermal synthesis of nanoporous cobalt oxides and their gas sensing properties

In this paper, the precursors were synthesized by microwave hydrothermal method using Co(NO₃)₂·6H₂O as raw material, CO(NH₂)₂ and KOH as precipitants, respectively. The precursors and calcined products were characterized by XRD, FESEM, and BET-BJH. The results show that both constituent and synthetic condition can determine the products morphology. When using KOH as precipitant, hollow Co₃O₄ nanorings were obtained whose precursor was synthesized at 140 °C for 3 h and calcined at 500 °C in air for 2 h. While using CO(NH)₂, Co₃O₄ like-nanochains were obtained whose precursor was synthesized at 110 °C for 1 h and calcined at 420 °C in air for 2 h, and Co₃O₄ nanosheets were obtained while their precursor was synthesized at 140 °C for 3 h and calcined at 500 °C in air for 2 h. The sensitivity test of Co₃O₄ to alcohol reveals that the hollow Co₃O₄ nanorings show the best sensitivity, porous Co₃O₄ like-nanochains are superior to that of the porous nanosheets.     

Preparation and electrochemical properties of nickel oxide as a supercapacitor electrode material

Hydrothermal synthesis has been introduced to fabricate NiO precursor at different temperatures, then nanostructured NiO with a distinct flake-like morphology was obtained via heating at low temperature. The NiO nanoflakes are 50-80 nm in width and 20 nm in thickness. The electrochemical capacitive characterization of the as-prepared NiO was studied in 2 M KOH electrolyte solution. The as-prepared NiO exhibits excellent cycle performance and keeps 91.6% initial capacity over 1000 charge-discharge cycles. Electrochemical impedance spectroscopy study reveals that the NiO electrode is controlled by the mass transfer limitation, and its internal resistance is 0.2 Ω. A specific capacitance approximate to 137.7 F g⁻¹ could be achieved at the current density of 0.2 A g⁻¹ in the potential window of 0-0.46 V in 2 M KOH electrolyte solution, due to higher surface area of NiO nanoflakes, which facilitates transport of electrolyte ions during rapid charge/discharge process. Due to higher surface area of NiO nanoflakes, which facilitates transport of electrolyte ions during rapid charge/discharge process.     

A facile method to prepare PbS nanorods

PbS nanorods with an average diameter of about 30 nm have been successfully prepared through a simple polyglycol-assisted route for the first time. The obtained PbS nanorods have been characterized using X-ray diffraction (XRD), transmission electron microscopy (TEM), and selected area electronic diffraction (SAED). Experiments show that polyglycol plays an important role for the control of the morphology of PbS nanostructures. The preliminary result of the UV-vis absorption spectrum of the PbS nanorods is also presented.     

FTIR study of the photocatalytic degradation of gaseous benzene over UV-irradiated TiO2 nanoballs synthesized by hydrothermal treatment in alkaline solution

In this study, photocatalysts of TiO₂ nanoballs were obtained via a hydrothermal treating of commercial P25 in alkaline solution, and then characterized with SEM, XRD, BET and surface photovoltage spectroscopy techniques. The UV-assisted photodegradation of gaseous benzene over P25 and the prepared TiO₂ nanoballs was monitored by an in situ infrared technique. The results demonstrated that the prepared TiO₂ nanoballs in anatase form were more active than commercial P25 in photocatalytic oxidation of gaseous benzene. The promoted activity of the hydrothermal-treated TiO₂ is attributed to the increasing specific surface area and larger band gap induced by the reduced crystallite size. The spectra of FTIR indicated that weakly adsorbed phenol was formed as the reaction progress. Hydroxyl groups on the surface of TiO₂ nanoballs are able to react with photo-produced phenol, which is then retained on the catalyst surface leading to the progressive deactivation of the catalyst in the gas-solid system.     

Synthesis and characterization of Co-Sn substituted barium ferrite particles by a reverse microemulsion technique

A series of Co-Sn substituted barium ferrite particles have been successfully synthesized by a reverse microemulsion technique. The effects of heteroatom contents and precipitating agents were investigated, respectively. It was found that the presence of heteroatoms could enhance lattice parameters, affect morphology evolution and modulate magnetic properties. Particularly, an unusual saturation magnetization (>70.0 emu/g) could be achieved under low heteroatoms concentration due to preferential occupation in specific sites. Precipitating agents played a critical role in forming barium ferrite phase, only sufficient precipitating agents could produce high-purity phase. Besides, this method is not limited in the synthesis of Co-Sn substituted barium ferrite, it can be extended to other heteroatoms, such as Ni-Zr and La, and resultant products also show well crystalline phase and unique magnetic properties.     

A novel solid-stabilized emulsion approach to CuO nanostructured microspheres

Nanostructured CuO microspheres were prepared by a novel solid-stabilized emulsion for the first time. SEM, TEM, XRD, size analysis and BET measurement were used to characterize the CuO microspheres. The average diameter of the CuO microspheres was 2.8 μm. The surfaces of the CuO microspheres were made of pin-like nanostructures with a pin diameter of 95 nm and a pin length of at least 600 nm. The XRD analysis indicated that the CuO nanostructured microspheres were of monoclinic lattice. The specific surface area of the CuO nanostructured microspheres was about 56.8 m²/g. A mechanism for the formation of the CuO microspheres with nanostructured surfaces was proposed.     

A template-free alcoholthermal route to Ti(Sn)-doped ZnO nanorods

Ti(Sn)-doped single-crystalline ZnO nanorods with an average diameter of 20 nm and length up to nearly 1 μm were synthesized by a facile ultrasonic irradiation-assisted alcoholthermal method without involving any templates. Photoluminescence spectra of the Ti-doped ZnO nanorods were measured at room temperature and three emitting bands, being a violet emission at 400-415 nm, a blue band at 450-470 nm and a green band at around 550 nm, were detected. The emission intensities of the Ti-doped ZnO nanorods enhance gradually with increasing the doping concentrations. As to the Sn-doped ZnO nanorods, the green emission shifts to 540 nm and the emission intensities increase first but decrease later with increasing the doping concentrations.     

Photocatalytic performance of Sn-doped TiO2 nanostructured thin films for photocatalytic degradation of malachite green dye under UV and VIS-lights

Sn-doped and undoped nano-TiO₂ particles have been synthesized by hydrotermal process without acid catalyst at 225 °C in 1 h. Nanostructure-TiO₂ based thin films, contain at different solid ratio of TiO₂ in coating, have been prepared on glass surfaces by spin-coating technique. The structure, surface morphology and optical properties of the thin films and the particles have been investigated by element analysis and XRD, BET and UV/VIS/NIR techniques. The photocatalytic performance of the films was tested for degradation of malachite green dye in solution under UV and VIS-lights. The results showed that the hydrothermally synthesized nano-TiO₂ particles are fully anatase crystalline form and are easily dispersed in water, the coated surfaces have nearly super-hydrophilic properties and, the doping of transition metal ion efficiently improved the photocatalytic performance of the TiO₂ thin film. The results also proved that malachite green is decomposed catalytically due to the pseudo first-order reaction kinetics.