Hydrogen Gas Sensing Based on SnO<Subscript>2</Subscript> Nanostructure Prepared by Sol–Gel Spin Coating Method

A novel H₂ gas sensor based on a SnO₂ nanostructure was operated at room temperature (RT) (25°C). The SnO₂ nanostructure was grown on Al₂O₃ substrates by a sol–gel spin coating method. The structural characteristics, surface morphology, and gas sensing properties of the SnO₂ nanostructure were investigated. Thin film annealing at 500°C produced a high-quality SnO₂ nanostructure with a crystallite size of 33.98 nm. A metal–semiconductor–metal gas sensor was fabricated using the SnO₂ nanostructure and palladium metal. The gas sensor exhibited a sensitivity of 2570% to 1000 ppm H₂ gas at RT. The sensing measurements for H₂ gas at different temperatures (RT to 125°C) were repeatable?for 50 min. Sensor sensitivity was tested under different H₂ concentrations (150 ppm, 250 ppm, 375 ppm, 500 ppm, and 1000 ppm) at different operating temperatures. Adding glycerin to the sol solution increased the porosity of the SnO₂ nanostructure surface, which increased the adsorption/desorption of gas molecules which leads to the high sensitivity of the sensor. Therefore, this H₂ gas sensor is a suitable?portable?RT gas sensor.     

Preparation of Bi<Subscript>0.85</Subscript>Nd<Subscript>0.15</Subscript>FeO<Subscript>3</Subscript> Nanotube Arrays by a Sol–Gel Template Method

Bi_0.85Nd_0.15FeO₃ (BNF) nanotube arrays were prepared by a sol–gel template method. The microstructure and phase were observed by scanning electron microscopy and transmission electron microscopy. Highly ordered nanotube arrays with BNF nanotubes of 200 nm diameter, 60 μm length, and 20 nm wall thickness were obtained. The BNF nanotube array capacitor showed ferroelectricity with a remanent polarization (2P _r) of 68.7 μC/cm² and a coercive electric field (2E _c) of 141.9 kV/cm at frequency of 1000 Hz. The leakage current behavior of the BNF nanotube array was dominated by an ohmic conduction mechanism at E < 30 kV/cm and a space-charge-limited current mechanism at E = 30 kV/cm to 200 kV/cm.     

Judd–Ofelt Analysis of Dy<Superscript>3+</Superscript>-Activated Aluminosilicate Glasses Prepared by Sol–Gel Method

Aluminosilicate (AS) glasses doped with different Dy³⁺ concentrations were synthesized via sol–gel method. Absorption, photoluminescence spectra and lifetime of this material have been studied. From analytical results of absorption spectra, the Judd–Ofelt (JO) parameters of prepared samples have been determined. These JO parameters combined with photoluminescence spectra have been used to evaluate transition probabilities (A_R), branching ratios (β) and the calculated oscillator strengths of AS:Dy³⁺ glasses. The radiative branching ratio of ⁴F_9/2 → ⁶H_13/2 transition has a minimum value at 62.2% for β_R which predicts that this transition in AS:Dy³⁺ glasses can give rise to lasing action. JO parameters show that the Ω₂ increases with the increasing of Dy³⁺ ion concentration due to the increased polarizability of the average coordination medium and decreased average symmetry.     

Enhanced Photocatalytic Activity of Two-Pot-Synthesized BiFeO<Subscript>3</Subscript>–ZnFe<Subscript>2</Subscript>O<Subscript>4</Subscript> Heterojunction Nanocomposite

BiFeO₃–ZnFe₂O₄ heterojunction nanocomposites have been produced by a chemical synthesis method using one- and two-pot approaches. X-ray diffraction patterns of as-calcined samples indicated formation of pure zinc ferrite (ZnFe₂O₄) and bismuth ferrite (BiFeO₃) phases, each retaining its crystal structure. Diffuse reflectance spectrometry was applied to calculate the optical bandgap of the photocatalysts, revealing values in the range from 2.03 eV to 2.17 eV, respectively. The maximum photodegradation of methylene blue of about 97% was achieved using two-pot-synthesized photocatalyst after 120 min of visible-light irradiation due to the higher probability of charge separation of photogenerated electron–hole pairs in the heterojunction structure. Photoluminescence spectra showed lower emission intensity of two-pot-synthesized photocatalyst, due to its lower recombination rate originating from greater charge separation.     

Sol–Gel Grown SnO<Subscript>2</Subscript> Nanoparticles: Evaluation of Structure,Morphology, and Raman Spectra

Tin oxide (SnO₂) nanoparticles (TONPs) were prepared using sol–gel method under different growth conditions. The influence of calcination temperature (450°C and 600°C) and molecular weight of polyethylene glycol (PEG 300 and PEG 4000) on the nanocrystallinity, surface morphology, and Raman spectra of as-prepared TONPs were evaluated. Variation of calcination temperature and dopant (sulfosuccinic acid, SA) was found to affect considerably the structure, surface morphology, and Raman activities of the TONPs. The size of TONPs estimated using Scherrer equation was discerned to be in the range of 15–32 nm. The observed intensity enhancement in the Raman vibrational modes at lower calcination temperature was attributed to the enlargement of TONPs size. The absorption of molecules at the TONPs surface led to a quenching in the A ₂ g and Eu Raman peaks. Raman peaks centered around 673 cm^?1, 799 cm^?1, 640 cm^?1 , and 432 cm^?1 corresponding to A1g, B2g, A1g, and Eg modes, respectively have manifested highest peaks intensity. Furthermore, the enhancement of the Eg mode due to the addition of SA dopant was ascribed to the Jahn–Teller distortion mechanism.     

Preparation and Ferroelectric Properties of Ho<Superscript>3+</Superscript>/Mo<Superscript>6+</Superscript> Cosubstituted Bi<Subscript>4</Subscript>Ti<Subscript>3</Subscript>O<Subscript>12</Subscript> Thin Films by Sol–Gel Method

We have prepared Ho³⁺/Mo⁶⁺ cosubstituted bismuth titanate [(Bi_3.6Ho_0.4)_3.99- Ti_2.985Mo_0.015O₁₂, BHTM] thin films on Pt/Ti/SiO₂/Si substrates using the sol–gel method. The crystal structure and morphology of the BHTM films were characterized. The BHTM samples show a single phase of Bi-layered Aurivillius structure and a dense microstructure. The dielectric constant and dielectric loss of the BHTM films were about 359 and 0.043, respectively, at a frequency of 1 MHz. The films exhibit 2P _r of 57.7 μC/cm² and 2E _c of 290.0 kV/cm at an applied field of 470 kV/cm, and have fatigue-free characteristics. They also showed good insulating behavior according to leakage current testing.     

Preparation by Poly(Acrylic Acid) Sol–Gel Method and Thermoelectric Properties of γ-Na<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>CoO<Subscript>2</Subscript> Bulk Materials

γ-Na _x CoO₂ single-phase powders have been synthesized by a poly(acrylic acid) (PAA) sol–gel (SG) method, and γ-Na _x CoO₂ bulk ceramic fabricated using spark plasma sintering. The effects of the PAA concentration on the sample phase composition and morphology were investigated. The thermoelectric properties of the γ-Na _x CoO₂ bulk ceramic were also studied. The results show that the PAA concentration did not significantly affect the crystalline phase of the product. However, agglomeration of γ-Na _x CoO₂ crystals was suppressed by the steric effect of PAA. The Na _x CoO₂ bulk ceramic obtained using the PAA SG method had higher crystallographic anisotropy, better chemical homogeneity, and higher density than the sample obtained by solid-state reaction (SSR), leading to improved thermoelectric performance. The PAA SG sample had power factor (in-plane PF = σS ²) of 0.61 mW m^?1 K^?2 and dimensionless figure of merit (ZT) along the in-plane direction of 0.19 at 900 K, higher than for the SSR sample (in-plane PF = 0.51 mW m^?1 K^?2, in-plane ZT = 0.17). These results demonstrate that a simple and feasible PAA SG method can be used for synthesis of Na _x CoO₂ ceramics with improved thermoelectric properties.     

Microstructure and Thermoelectric Transport Properties of Type I Clathrates Ba<Subscript>8</Subscript>Sb<Subscript>2</Subscript>Ga<Subscript>14</Subscript>Ge<Subscript>30</Subscript> Prepared by Ultrarapid Solidification Process

Type I clathrate bulk materials Ba₈Sb₂Ga₁₄Ge₃₀ were prepared by the melt spinning (MS) technique combined with the spark plasma sintering (SPS) method. The microstructure and thermoelectric transport properties of the compounds were investigated. The results show that the grain size decreases greatly compared with materials obtained by the traditional melting and SPS method. The electrical conductivity increases greatly and the lattice thermal conductivity decreases significantly with increasing roller linear speed. The maximum thermoelectric dimensionless figure of merit ZT of 1.05 is obtained at 950 K for the sample prepared by melt spinning with a roller linear speed of 40 m/s.     

Conductivity of Ga<Subscript>2</Subscript>O<Subscript>3</Subscript>–GaAs Heterojunctions

The effect of annealing in argon at temperatures of T_an = 700–900°C on the I–V characteristics of metal–Ga₂O₃–GaAs structures is investigated. Samples are prepared by the thermal deposition of Ga₂O₃ powder onto GaAs wafers with a donor concentration of N _d = 2 × 10¹⁶ cm^–3. To measure theI–V characteristics, V/Ni metal electrodes are deposited: the upper electrode (gate) is formed on the Ga₂O₃ film through masks with an area of S _k = 1.04 × 10^–2 cm² and the lower electrode in the form of a continuous metallic film is deposited onto GaAs. After annealing in argon at T_an ≥ 700°C, the Ga₂O₃-n-GaAs structures acquire the properties of isotype n-heterojunctions. It is demonstrated that the conductivity of the structures at positive gate potentials is determined by the thermionic emission from GaAs to Ga₂O₃. Under negative biases, current growth with an increase in the voltage and temperature is caused by field-assisted thermal emission in gallium arsenide. In the range of high electric fields, electron phonon-assisted tunneling through the top of the potential barrier is dominant. High-temperature annealing does not change the electron density in the oxide film, but affects the energy density of surface states at the GaAs–Ga₂O₃ interface.     

Luminescence Properties of Cobalt-Doped ZnO Films Prepared by Sol–Gel Method

Pure ZnO and Co-doped ZnO films have been deposited on coverslip substrates by sol–gel spin coating. The morphological, structural, and optical properties of the films were investigated. The microstructure of the ZnO films became increasingly fine and the crystalline size decreased with Co doping. Analysis of x-ray diffraction (XRD) and Raman spectra reveals that Co²⁺ ions are substituted for Zn²⁺ ions in the ZnO lattice without changing its wurtzite structure. Co doping induces a decrease of the band-gap energy and fluorescence quenching of the emission bands. The spectra related to transitions within the tetrahedral Co²⁺ ions in the ZnO host crystal were observed in absorption and luminescence spectra. Photoluminescence (PL) spectra under different excitation energies and PL excitation spectra for the visible emissions suggest that the orange–red emission and green emission could be related to interstitial zinc (Zn_i) shallow donors and oxygen vacancy (V _O) deep donors, respectively. The red emission of Co-doped ZnO film could be assigned to the radiative transitions within the tetrahedral Co²⁺ ions in the ZnO host crystal after band-to-band excitation. A consistent explanation for the pure and Co-doped ZnO films is that the red emission under the excitation energy below the band gap is probably associated with extended Zn_i states.     

Synthesis and Electrical Properties of γ-Na<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript>Co<Subscript>2</Subscript>O<Subscript>4</Subscript> via a Citrate Sol–Gel Method with Polyethylene Glycol 400

In this work, a citrate sol–gel method (Sol–Gel) with polyethylene glycol 400 (Sol-Gel-PEG400) was developed to prepare γ-Na _x Co₂O₄ by using sodium and cobalt nitrates as the raw materials, citric acid as a complexing agent, and PEG400 as a dispersant. At 800°C, single-phase γ-Na _x Co₂O₄ crystals were obtained using Sol-Gel-PEG400. With the addition of 1 vol.% PEG400, smaller, flaky particles exhibited a well-tiled structure along the plane direction of the flaky particles. Moreover, polycrystalline sintered bulk γ-Na _x Co₂O₄ with more highly oriented crystals and greater compact density was fabricated using the Sol-Gel-PEG400 synthesized powders compared with the powders synthesized by citrate Sol–Gel. The electrical conductivity (σ) values of Sol-Gel-PEG400 samples were higher than those of Sol–Gel samples between 400 K and 900 K. The σ value of Sol-Gel-PEG400 increased to 3.13 × 10⁴ Sm⁻¹ at 400 K and to 1.84 × 10⁴ Sm⁻¹ at 900 K. Between 400 K and 850 K, the Seebeck coefficient (α) values of Sol-Gel-PEG400 samples were slightly lower than those of Sol–Gel samples. Near 900 K, the α values of these two methods were nearly equal, at 164 μV K⁻¹. Between 400 K and 900 K, the power factor (P) of Sol-Gel-PEG400 was evidently larger than that of Sol–Gel.     

Conduction in titanium dioxide films and metal–TiO<Subscript>2</Subscript>–Si structures

The effect of the annealing of titanium oxide films on the electrical properties of metal–TiO₂–n-Si structures is investigated. It is shown that, regardless of the annealing temperature, the conductivity of the structures at positive gate potentials is determined by the space-charge-limited current in the insulator with traps exponentially distributed in terms of energy. At negative gate potentials, the main contribution to the current is provided by the generation of electron–hole pairs in the space-charge region in silicon. The properties of the TiO₂/n-Si interface depend on the structure and phase state of the oxide film, which are determined by the annealing temperature.     

Interdiffusion and phase formation in the Fe–TiO<Subscript>2</Subscript> thin-film system

The interaction of magnetron-sputtered metal iron with titanium-oxide films upon isothermal vacuum annealing is studied by X-ray phase analysis, secondary-ion mass spectrometry, atomic-force microscopy, and mathematical simulation. A mechanism for the formation of complex oxides at grain boundaries is suggested. The mechanism is based on the reaction diffusion of metal iron into titanium oxide. A quantitative model of reaction interdiffusion in two-layer polycrystalline metal–oxide film systems with limited component solubility is developed. From numerical analysis of the experimental distributions of the metal concentrations in the Fe–TiO₂ film system, the individual diffusion coefficients are determined. It is found that, under the conditions of vacuum annealing at 1073 K, the diffusion coefficients of iron and titanium are 8.0 × 10^–13 and 3.0 × 10^–15 cm² s^–1, respectively.     

Photoluminescence and excitation features of Nd<Superscript>3+</Superscript> ions in (La<Subscript>0.97</Subscript>Nd<Subscript>0.03</Subscript>)<Subscript>2</Subscript>S<Subscript>3</Subscript> · 2Ga<Subscript>2</Subscript>O<Subscript>3</Subscript> glasses

A combined study of the spectral photoluminescence distribution and excitation spectra of photoluminescence in La₂S₃ · 2Ga₂O₃ and (La_0.97Nd_0.03)₂S₃ · 2Ga₂O₃ glasses, along with the study of the transmission spectra of these glasses, was carried out. The radiative channel was ascertained to be the main channel for the energy transfer from the host matrix to the Nd³⁺ ions upon excitation of the glasses with light at a wavelength of the fundamental absorption band. Oxygen centers with the level E _c -2.0 eV act as sensitizing agents. The structural disordering of the glass host increases the variance in the magnitude of splitting of the multiplet levels from the 4f electronic states of the Nd³⁺ ion. This promotes nonradiative relaxation of the electrons from excited states to the laser ⁴F_3/2 level. The (La_0.97Nd_0.03)₂S₃ · 2Ga₂O₃ glasses can be considered as promising laser materials for obtaining the stimulated emission of radiation of Nd³⁺ ions under an optical pump in the range of the fundamental absorption band of the glass.     

Structure and Properties of Nanostructured YBa<Subscript>2</Subscript>Cu<Subscript>3</Subscript>O<Subscript>7–δ</Subscript>, BiFeO<Subscript>3</Subscript>, and Fe<Subscript>3</Subscript>O<Subscript>4</Subscript>

The development of new nanostructured materials based on YBa₂Cu₃O_7–δ, BiFeO₃, and Fe₃O₄ compounds is considered. The structure, morphology, and properties of these materials are studied. The possibilities of fabricating YBa₂Cu₃O_7–δ ceramics with given densities from nanopowders in a single stage by an energy efficient method and growing superconducting films of the same composition on a silicon substrate (on a SiO₂ layer) are demonstrated. The technique for fabricating BiFeO₃ nanopowder, making it possible to obtain nanostructured ceramics without additional accompanied phases commonly forming during BiFeO₃ synthesis is developed. Two methods of the single-stage synthesis of Fe₃O₄ nanopowder are presented: burning of nitrate-organic precursors and the electrochemical three-electrode method in which one of the electrodes, i.e., an anode containing scrap iron and slurry, is used as an expendable material.     

Thermal Conductivity Reduction in CoSb<Subscript>3</Subscript>–CeO<Subscript>2</Subscript> Nanocomposites

CoSb₃ + x% CeO₂ nanocomposites (x = 1, 3, 5) were synthesized by ball-milling and spark plasma sintering. Scanning electron microscopy showed that some CeO₂ nano-inclusions sit at the boundaries of CoSb₃ grains. These inclusions also reduce the sizes of the CoSb₃ grains and crystallites by inhibiting their growth during sintering. Hall-effect measurements show that the CeO₂ inclusions modify the charge-carrier concentration in CoSb₃. The variations of the electrical resistivity for the 1% and 3% CeO₂ samples can at least partially be attributed to these modifications of the carrier concentration. Nonetheless, the resistivity increase in the 5% CeO₂ sample can unambiguously be ascribed to the presence of the CeO₂ inclusions. Thermal conductivity is systematically reduced (by more than 15% at 300 K) upon CeO₂ addition. Phonon diffusion by the increased number of CoSb₃ grain boundaries is one of the mechanisms involved in this reduction.     

Deposition of heteroepitaxial layers of topological insulator Bi<Subscript>2</Subscript>Se<Subscript>3</Subscript> in the trimethylbismuth–isopropylselenide–hydrogen system on the (0001) Al<Subscript>2</Subscript>O<Subscript>3</Subscript> and (100) GaAs substrates

Thin solid layers that are formed upon heating of the gaseous trimethylbismuth–isopropylselenide–hydrogen system on the (0001) Al₂O₃ and singular and vicinal (100) GaAs surfaces are studied. The conditions for deposition of metal Bi and phases of Bi₄Se₃, BiSe, and topological insulator Bi₂Se₃ using the MOCVD method are determined. Pure metastable phase BiSe is obtained for the first time. Bi₂Se₃ films with a thickness of no less than 200 nm, a relatively low volume concentration of 3 ×10¹⁸ cm^–3, and a high mobility of carriers at 300 K (1000 cm² V^–1 s^–1) are fabricated.     

Plasmon–phonon coupling in the infrared reflectance spectra of Bi<Subscript>2</Subscript>Se<Subscript>3</Subscript> films

The results of studies of optical reflection in the far- and mid-infrared spectral regions are reported. The reflectance of five Bi₂Se₃ topological insulator films grown by molecular-beam epitaxy on Si(111) substrates is measured. The characteristic parameters of phonons and plasmons are determined by means of dispersion analysis for multilayer structures. It is found that the plasma frequency in a layer close to the Si–film interface is noticeably higher than that in the film bulk. Calculations of the loss function show that plasmon–phonon coupling plays an important role in Bi₂Se₃ films. The attenuated total internal reflection method is used to determine the frequency of the surface plasmon–phonon mode.