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Synthesis of Cu?O/CuO Nanocrystals and Their Application to H?S Sensing.

ABSTRACT: Semiconducting metal oxide nanocrystals are an important class of materials that have versatile applications because of their useful properties and high stability. Here, we developed a simple route to synthesize nanocrystals (NCs) of copper oxides such as Cu?O and CuO using a hot-soap method, and applied them to H?S sensing. Cu?O NCs were synthesized by simply heating a copper precursor in oleylamine in the presence of diol at 160 °C under an Ar flow. X-ray diffractometry (XRD), dynamic light scattering (DLS), and transmission electron microscopy (TEM) results indicated the formation of monodispersed Cu?O NCs having approximately 5 nm in crystallite size and 12 nm in colloidal size. The conversion of the Cu?O NCs to CuO NCs was undertaken by straightforward air oxidation at room temperature, as confirmed by XRD and UV-vis analyses. A thin film Cu?O NC sensor fabricated by spin coating showed responses to H?S in dilute concentrations (1?8 ppm) at 50?150 °C, but the stability was poor because of the formation of metallic Cu?S in a H?S atmosphere. We found that Pd loading improved the stability of the sensor response. The Pd-loaded Cu?O NC sensor exhibited reproducible responses to H?S at 200 °C. Based on the gas sensing mechanism, it is suggested that Pd loading facilitates the reaction of adsorbed oxygen with H?S and suppresses the irreversible formation of Cu?S.

SUBMITTER: Mikami K

PROVIDER: S-EPMC6339020 | biostudies-literature | 2019 Jan

REPOSITORIES: biostudies-literature

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Synthesis of Cu₂O/CuO Nanocrystals and Their Application to H₂S Sensing.

Mikami Kazuki K Kido Yuta Y Akaishi Yuji Y Quitain Armando A Kida Tetsuya T

Sensors (Basel, Switzerland) 20190108 1

Semiconducting metal oxide nanocrystals are an important class of materials that have versatile applications because of their useful properties and high stability. Here, we developed a simple route to synthesize nanocrystals (NCs) of copper oxides such as Cu₂O and CuO using a hot-soap method, and applied them to H₂S sensing. Cu₂O NCs were synthesized by simply heating a copper precursor in oleylamine in the presence of diol at 160 °C under an Ar flow. X-ray diffractometry (XRD), dynamic light sc ...[more]

PMID: 30626139

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Project description:The synthesis of optoelectrically enhanced nanomaterials should be continuously improved by employing time- and energy-saving techniques. The porous zinc oxide (ZnO) and copper-doped ZnO nanocomposites (NCs) were synthesized by the time- and energy-efficient solution combustion synthesis (SCS) approach. In this SCS approach, once the precursor-surfactant complex ignition point is reached, the reaction starts and ends within a short time without the need for any external energy. The TGA-DTA analysis confirmed that 500 °C was the point at which stable metal oxide was obtained. The doping and heterojunction strategy improved the optoelectric properties of the NCs more than the individual constituents, which then enhanced the materials' charge transfer and optical absorption capabilities. The porosity, nanoscale crystallite size (15-50 nm), and formation of Cu/CuO-ZnO NCs materials were confirmed from the XRD, SEM, and TEM/HRTEM analyses. The obtained d-spacing values of 0.275 and 0.234 nm confirm the formation of ZnO and CuO crystals, respectively. The decrease in photoluminescence intensity for the doped NCs corroborates a reduction in electron-hole recombination. On the Mott-Schottky analysis, the positive slope for ZnO confirms the n-type character, while the negative and positive slopes of the NCs confirm the p- and n-type characters, respectively. A diffusion-controlled type of charge transfer process on the electrode surface was confirmed from the cyclic voltammetric analysis. Thus, the overall analysis shows the applicability of the less expensive and more efficient SCS for several applications, such as catalysis and sensors. To confirm this, an organic catalytic reduction reaction of 4-nitrophenol to 4-aminophenol was tested. Within three and a half minutes, the catalytic reduction result showed the great potential of NCs over ZnO NPs. Thus, the energy- and time-saving SCS approach has a great future outlook as an industrial pollutant catalytic reduction application.

Project description:Augmenting the oriented attachment (OA) crystal growth phenomena, herein, we demonstrate fabrication of ultrathin CuO nanowires from self-assembled one-dimensional (1D) nanowires of Cu(OH)2 nanocrystals. A facile environmentally benign sol-gel approach, which utilizes base-catalyzed hydrolysis followed by directed self-assembly and crystal growth of nanocrystals, is developed to prepare Cu(OH)2 nanowires. The sol of Cu(OH)2 nanocrystals shows aggregative self-assembly guided by the OA crystal growth process to form ultrathin Cu(OH)2 nanowires, with an average length of 675 ± 4 nm and diameter of 6 ± 2 nm. The time-dependent UV-visible spectral traces, along with real-time imaging of nanocrystals self-assembly and growth under the transmission electron microscope, are evidenced the concept of the OA crystal growth directed self-assembly, yielding 1D colloidal nanoarrays of Cu(OH)2. The powder XRD traces collected during the self-assembly and crystal growth process reveal the directional aggregative crystal growth along the facet of [001], confirming the OA directed crystal growth and fusion of nanocrystals to yield 1D nanostructures. The gradual blue-shift in optical absorption maxima from 770 nm in initial precursor solution, to 670 nm for Cu(OH)2 nanocrystals sol, and finally to 647 nm for self-assembled 1D Cu(OH)2 nanowires have further evidenced the formation of Cu(OH)2 nanowires. Upon subjecting self-assembled Cu(OH)2 nanowires for post-annealing treatment, ultrathin CuO nanowires with average length of 7 ± 0.50 μm and diameter of 27 ± 2 nm is obtained in high purity. The experimental powder XRD patterns of Cu(OH)2 and CuO nanowires match the simulated XRD patterns, indexing the crystal unit cell structures to orthorhombic and monoclinic, respectively. The tailored narrow optical band gaps for Cu(OH)2 and CuO nanowires are found to be 1.51 eV and 1.10 eV. The theoretical band gap predicted for Cu(OH)2 nanowires is 1.52 eV and is in good agreement with its optical band gap, whereas theoretical band computed for CuO nanowires is 0.13 eV lower than from its optical band gap.

Dataset Information

Synthesis of Cu?O/CuO Nanocrystals and Their Application to H?S Sensing.

Publications

Synthesis of Cu₂O/CuO Nanocrystals and Their Application to H₂S Sensing.

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