Chaikarn Liewhiran

Electrolytically Exfoliated Graphene-Loaded Flame-Made Ni-Doped SnO2 Composite Film for Acetone Sensing

In this work, flame-spray-made SnO2 nanoparticles are systematically studied by doping with 0.1-2 wt % nickel (Ni) and loading with 0.1-5 wt % electrolytically exfoliated graphene for acetone-sensing applications. The sensing films (∼12-18 μm in thickness) were prepared by a spin-coating technique on Au/Al2O3 substrates and evaluated for acetone-sensing performances at operating temperatures ranging from 150 to 350 °C in dry air. Characterizations by X-ray diffraction, transmission/scanning electron microscopy, Brunauer-Emmett-Teller analysis, X-ray photoelectron spectroscopy and Raman spectroscopy demonstrated that Ni-doped SnO2 nanostructures had a spheriodal morphology with a polycrystalline tetragonal SnO2 phase, and Ni was confirmed to form a solid solution with SnO2 lattice while graphene in the sensing film after annealing and testing still retained its high-quality nonoxidized form. Gas-sensing results showed that SnO2 sensing film with 0.1 wt % Ni-doping concentration exhibited an optimal response of 54.2 and a short response time of ∼13 s toward 200 ppm acetone at an optimal operating temperature of 350 °C. The additional loading of graphene at 5 wt % into 0.1 wt % Ni-doped SnO2 led to a drastic response enhancement to 169.7 with a very short response time of ∼5.4 s at 200 ppm acetone and 350 °C. The superior gas sensing performances of Ni-doped SnO2 nanoparticles loaded with graphene may be attributed to the large specific surface area of the composite structure, specifically the high interaction rate between acetone vapor and graphene-Ni-doped SnO2 nanoparticles interfaces and high electronic conductivity of graphene. Therefore, the 5 wt % graphene loaded 0.1 wt % Ni-doped SnO2 sensor is a promising candidate for fast, sensitive and selective detection of acetone.

Sensing Characteristics of Flame-Spray-Made Pt/ZnO Thick Films as H(2) Gas Sensor.

Hydrogen sensing of thick films of nanoparticles of pristine, 0.2, 1.0 and 2.0 atomic percentage of Pt concentration doped ZnO were investigated. ZnO nanoparticles doped with 0.2–2.0 at.% Pt were successfully produced in a single step by flame spray pyrolysis (FSP) technique using zinc naphthenate and platinum(II) acetylacetonate as precursors dissolved in xylene. The particle properties were analyzed by XRD, BET, SEM and TEM. Under the 5/5 (precursor/oxygen) flame condition, ZnO nanoparticles and nanorods were observed. The crystallite sizes of ZnO spheroidal and hexagonal particles were found to be ranging from 5 to 20 nm while ZnO nanorods were seen to be 5–20 nm wide and 20–40 nm long. ZnO nanoparticles paste composed of ethyl cellulose and terpineol as binder and solvent respectively was coated on Al2O3 substrate interdigitated with gold electrodes to form thin films by spin coating technique. The thin film morphology was analyzed by SEM technique. The gas sensing properties toward hydrogen (H2) was found that the 0.2 at.% Pt/ZnO sensing film showed an optimum H2 sensitivity of ∼164 at hydrogen concentration in air of 1 volume% at 300 °C and a low hydrogen detection limit of 50 ppm at 300 °C operating temperature.

H2 Sensing Response of Flame-Spray-Made Ru/SnO2 Thick Films Fabricated from Spin-Coated Nanoparticles

High specific surface area (SSABET: 141.6 m2/g) SnO2 nanoparticles doped with 0.2–3 wt% Ru were successfully produced in a single step by flame spray pyrolysis (FSP). The phase and crystallite size were analyzed by XRD. The specific surface area (SSABET) of the nanoparticles was measured by nitrogen adsorption (BET analysis). As the Ru concentration increased, the SSABET was found to linearly decrease, while the average BET-equivalent particle diameter (dBET) increased. FSP yielded small Ru particles attached to the surface of the supporting SnO2 nanoparticles, indicating a high SSABET. The morphology and accurate size of the primary particles were further investigated by TEM. The crystallite sizes of the spherical, hexagonal, and rectangular SnO2 particles were in the range of 3–10 nm. SnO2 nanorods were found to range from 3–5 nm in width and 5–20 nm in length. Sensing films were prepared by the spin coating technique. The gas sensing of H2 (500–10,000 ppm) was studied at the operating temperatures ranging from 200–350 °C in presence of dry air. After the sensing tests, the morphology and the cross-section of sensing film were analyzed by SEM and EDS analyses. The 0.2%Ru-dispersed on SnO2 sensing film showed the highest sensitivity and a very fast response time (6 s) compared to a pure SnO2 sensing film, with a highest H2 concentration of 1 vol% at 350 °C and a low H2 detection limit of 500 ppm at 200 °C.

Ultrasensitive NO2 Sensor Based on Ohmic Metal–Semiconductor Interfaces of Electrolytically Exfoliated Graphene/Flame-Spray-Made SnO2 Nanoparticles Composite Operating at Low Temperatures

In this work, flame-spray-made undoped SnO2 nanoparticles were loaded with 0.1-5 wt % electrolytically exfoliated graphene and systematically studied for NO2 sensing at low working temperatures. Characterizations by X-ray diffraction, transmission/scanning electron microscopy, and Raman and X-ray photoelectron spectroscopy indicated that high-quality multilayer graphene sheets with low oxygen content were widely distributed within spheriodal nanoparticles having polycrystalline tetragonal SnO2 phase. The 10-20 μm thick sensing films fabricated by spin coating on Au/Al2O3 substrates were tested toward NO2 at operating temperatures ranging from 25 to 350 °C in dry air. Gas-sensing results showed that the optimal graphene loading level of 0.5 wt % provided an ultrahigh response of 26,342 toward 5 ppm of NO2 with a short response time of 13 s and good recovery stabilization at a low optimal operating temperature of 150 °C. In addition, the optimal sensor also displayed high sensor response and relatively short response time of 171 and 7 min toward 5 ppm of NO2 at room temperature (25 °C). Furthermore, the sensors displayed very high NO2 selectivity against H2S, NH3, C2H5OH, H2, and H2O. Detailed mechanisms for the drastic NO2 response enhancement by graphene were proposed on the basis of the formation of graphene-undoped SnO2 ohmic metal-semiconductor junctions and accessible interfaces of graphene-SnO2 nanoparticles. Therefore, the electrolytically exfoliated graphene-loaded FSP-made SnO2 sensor is a highly promising candidate for fast, sensitive, and selective detection of NO2 at low operating temperatures.

Flame-Made Nb-Doped TiO2 Ethanol and Acetone Sensors

Undoped TiO2 and TiO2 nanoparticles doped with 1–5 at.% Nb were successfully produced in a single step by flame spray pyrolysis (FSP). The phase and crystallite size were analyzed by XRD. The BET surface area (SSABET) of the nanoparticles was measured by nitrogen adsorption. The trend of SSABET on the doping samples increased and the BET equivalent particle diameter (dBET) (rutile) increased with the higher Nb-doping concentrations while dBET (anatase) remained the same. The morphology and accurate size of the primary particles were further investigated by high-resolution transmission electron microscopy (HRTEM). The crystallite sizes of undoped and Nb-doped TiO2 spherical were in the range of 10–20 nm. The sensing films were prepared by spin coating technique. The mixing sample was spin-coated onto the Al2O3 substrates interdigitated with Au electrodes. The gas sensing of acetone (25–400 ppm) was studied at operating temperatures ranging from 300–400 °C in dry air, while the gas sensing of ethanol (50–1,000 ppm) was studied at operating temperatures ranging from 250–400 °C in dry air.

Flame-spray-made undoped zinc oxide films for gas sensing applications.

Using zinc naphthenate dissolved in xylene as a precursor undoped ZnO nanopowders were synthesized by the flame spray pyrolysis technique. The average diameter and length of ZnO spherical and hexagonal particles were in the range of 5 to 20 nm, while ZnO nanorods were found to be 5–20 nm wide and 20–40 nm long, under 5/5 (precursor/oxygen) flame conditions. The gas sensitivity of the undoped ZnO nanopowders towards 50 ppm of NO2, C2H5OH and SO2 were found to be 33, 7 and 3, respectively. The sensors showed a great selectivity towards NO2 at high working temperature (at 300 °C), while small resistance variations were observed for C2H5OH and SO2, respectively.

Synthesis of thermally spherical CuO nanoparticles

Copper oxide (CuO) nanoparticles were successfully synthesized by a thermal method. The CuO nanoparticles were further characterized by thermogravimetric analysis (TGA), differential thermal analysis (DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (EDS), and high resolution transmission electron microscopy (HRTEM), respectively. The specific surface area (SSABET) of CuO nanoparticles was determined by nitrogen adsorption. The SSABET was found to be 99.67m2/g (dBET of 9.5 nm). The average diameter of the spherical CuO nanoparticles was approximately 6-9 nm.

Effect of Palladium on Photocatalytic Activity of SnO2 Nanoparticles

SnO2 nanoparticles were successfully synthesized with either the presence (PS) or absence (NPS) of the Broussonetia papyrifera (L.) Vent Pulp as the dispersant by the precipitation coupling with the thermal decomposition methods using tin tetrachloride pentahydrate (Sn4Cl.5H2O) and ammonium hydroxide (NH4OH) as the starting material and precipitant respectively. The pulp was soaked in SnCl4 solution and NH4OH was slowly added dropwise. The white gelable precipitate of Sn(OH)4 was obtained. Afterward, the white precipitate was filtered and washed until it was free from chloride. The white precipitate was then dried at 80°C for 24h and calcined for 1h at 600°C, 650°C, and 700°C respectively. The synthesized products were characterized by X-ray diffraction (XRD), transmission electron microscope (TEM) and Brunauer-Emmett-Teller (BET) measurement of specific surface area. The crystallite sizes of SnO2 nanoparticles with the presence and absence of the pulp were found to be ranging from 5-15 nm and 5-30 nm respectively. The specific surface areas (SSABET) were 62.53 m2/g and 26.60 m2/g for PS and NPS samples respectively. SnO2 nanoparticles were doped with palladium in the range from 0.25-1.00 mol% by the impregnation method. The photocatalytic activity of SnO2 and Pd-doped SnO2 nanoparticles were investigated for the degradation of sucrose and glucose under UVA-light irradiation. The results showed that the photocatalytic activity of Pd-doped SnO2 was higher than pure SnO2 and the best photocatalytic activity for the degradation of sucrose and glucose were obtained in the case of Pd-doped SnO2 nanoparticles with 0.5 mol % and 1.0 mol % Pd loading respectively.

Hydrogen sensors based on zinc oxide nanoparticles

Pure ZnO, pure MgO and 5 wt%MgO/ZnO nanocomposites were produced by flame spray pyrolysis (FSP) in a single step using zinc naphthenate and magnesium acetate tetrahydrate as Zn and Mg precursors. The particle properties were analyzed by XRD, BET and TEM analyses. The sensing films were prepared by mixing the nanoparticles into an organic paste composed of ethyl cellulose and terpineol as a vehicle binder and solvent, respectively. The resulting paste was spin-coated on Al2O3 substrates interdigitated Au electrodes. The gas sensing of H2 concentration ranging from 0.5–1 vol% was studied at 300°C in dry air. The 5 wt% MgO/ZnO nanocomposites film showed higher sensitivity. The sensitivity increased and the response time decreased with increasing H2 concentrations.

High Performance Ethanol Sensor for Control Drunken Driving Based on Flame-made ZnO Nanoparticles

ZnO nanoparticles were produced by FSP using zinc naphthenate as a precursor dissolved in toluene/acetonitrile (80/20 vol%). The phase and crystallite size were analyzed by X-ray diffraction (XRD), and the specific surface area (SSA) of the nanoparticles was measured by nitrogen adsorption (BET analysis). The ZnO particle size and morphologies was further investigated by transmission electron microscopy (TEM) revealing spheroidal, hexagonal, and rod-like morphologies. The crystallite sizes of ZnO spheroidal and hexagonal particles were in the range of 10-20 nm. ZnO nanorods were found to be ranging from 10-20 nm in width and 20-50 nm in length. Sensing films were produced by mixing the particles into an organic paste composed of terpineol and ethyl cellulose as a vehicle binder. The paste was doctor-bladed onto Al2O3 substrates interdigitated with Au electrodes. The morphology of the sensing films was analyzed by scanning electron microscopy (SEM). The gas sensing of ethanol (25-250 ppm) was studied at 400 degC in dry air. The oxidation of ethanol on the surface of the semiconductor was confirmed by mass spectroscopy (MS). Thick (5 mum) ZnO films showed high sensitivity and fast response times (within seconds). The sensitivity increased and the response time decreased with increasing ethanol concentration. These concentrations (25-250 ppm) were corresponded to be almost in the same range with detection limit of concentration for human breath analyzer. These sensor can be performed an ethanol sensing device that could be employed for control of drunken driving.