Preparation of meso-porous SnO2 fibers with enhanced sensitivity for n-butanol

Meso-porous SnO₂ fibers were synthesized using a solvothermal method with metaplexis fruit as the bio-template. The products were characterized by powder X-ray diffraction, high resolution scanning electron microscopy, transmission electron microscopy and nitrogen adsorption/desorption measurements. Results show that SnO₂ fibers present a high specific surface area of 73.665 m²/g and a meso-porous structure with the pore size of 7.821 nm, and the crystal size of SnO₂ is about 6.5 ± 0.5 nm. The gas sensing performance of the prepared SnO₂ fibers toward several volatile organic compounds was investigated. The results show that the meso-porous SnO₂ fibers were highly sensitive and selective to n-butanol.     

Influence of Pd-loading on gas sensing characteristics of SnO2 thick films

Nanocrystalline pristine and 0.5, 1.5 and 3.0 wt% Pd loaded SnO₂ were synthesized by a facile co-precipitation route. These powders were screen-printed on alumina substrates to form thick films to investigate their gas sensing properties. The crystal structure and morphology of different samples were characterized by using X-ray diffraction, scanning electron microscopy and transmission electron microscopy techniques. The 3.0 wt% Pd:SnO₂ showed response of 85% toward 100 ppm of LPG at operating temperature of 250 °C with fast response (8 s) and quick recovery time (24 s). The high response toward LPG on Pd loading can be attributed to lowering of crystallite size (9 nm) as well as the role of Pd particles in exhibiting spill-over mechanism on the SnO₂ surface. Also selectivity of 3.0 wt% Pd:SnO₂ toward LPG was confirmed by measuring its response to other reducing gases like acetone (CH₃COCH₃), ethanol (C₂H₅OH) and ammonia (NH₃) at optimum operating temperature.     

SnO2 nano-spheres/graphene hybrid for high-performance lithium ion battery anodes

SnO₂ nano-spheres/graphene composite was fabricated via a simple one-step hydrothermal method with graphene oxide and SnCl₄·5H₂O as the precursors. The composite was characterized by X-ray diffraction, field-emission scanning electron microscopy, transmission electron microscopy and surface area measurement. It is shown that fine SnO₂ nano-spheres with an average size of 50–100 nm could be homogeneously deposited on graphene nano-sheets layer by layer. The structural feature enabled SnO₂ nano-spheres/graphene hybird as an excellent anode material in lithium ion battery. The composite possesses 1306 mA h g^?1 of initial discharge capacity and good capacity retention of 594 mA h g^?1 up to the 50th cycle at a current density of 100 mA g^?1. These results indicate that the composite is a promising anode material in high-performance lithium ion batteries.     

Preparation and electrochemical performance of SnO2@carbon nanotube core–shell structure composites as anode material for lithium-ion batteries

Carbon nanotube-encapsulated SnO₂ (SnO₂@CNT) core–shell composite anode materials are prepared by chemical activation of carbon nanotubes (CNTs) and wet chemical filling. The results of X-ray diffraction and transmission electron microscopy measurements indicate that SnO₂ is filled into the interior hollow core of CNTs and exists as small nanoparticles with diameter of about 6 nm. The SnO₂@CNT composites exhibit enhanced electrochemical performance at various current densities when used as the anode material for lithium-ion batteries. At 0.2 mA cm^?2 (0.1C), the sample containing wt. 65% of SnO₂ displays a reversible specific capacity of 829.5 mAh g^?1 and maintains 627.8 mAh g^?1 after 50 cycles. When the current density is 1.0, 2.0, and 4.0 mA cm^?2 (about 0.5, 1.0, and 2.0C), the composite electrode still exhibits capacity retention of 563, 507 and 380 mAh g^?1, respectively. The capacity retention of our SnO₂@CNT composites is much higher than previously reported values for a SnO₂/CNT composite with the same filling yield. The excellent lithium storage and rate capacity performance of SnO₂@CNT core–shell composites make it a promising anode material for lithium-ion batteries.     

Free-standing single-walled carbon nanotube/SnO2 anode paper for flexible lithium-ion batteries

Free-standing single-walled carbon nanotube/SnO₂ (SWCNT/SnO₂) anode paper was prepared by vacuum filtration of SWCNT/SnO₂ hybrid material which was synthesized by the polyol method. From field emission scanning electron microscopy and transmission electron microscopy, the CNTs form a three-dimensional nanoporous network, in which ultra-fine SnO₂ nanoparticles, which had crystallite sizes of less than 5 nm, were distributed, predominately as groups of nanoparticles on the surfaces of single walled CNT bundles. Electrochemical measurements demonstrated that the anode paper with 34 wt.% SnO₂ had excellent cyclic retention, with the high specific capacity of 454 mAh g^?1 beyond 100 cycles at a current density of 25 mA g^?1, much higher than that of the corresponding pristine CNT paper. The SWCNTs could act as a flexible mechanical support for strain release, offering an efficient electrically conducting channel, while the nanosized SnO₂ provides the high capacity. The SWCNT/SnO₂ flexible electrodes can be bent to extremely small radii of curvature and still function well, despite a marginal decrease in the conductivity of the cell. The electrochemical response is maintained in the initial and further cycling process. Such capabilities demonstrate that this model hold great promise for applications requiring flexible and bendable Li-ion batteries.     

Essential Macleod Program (EMP) simulated fabrication of high quality Zn:SnO2/Ag/Zn:SnO2 multilayer transparent conducting electrode on flexible substrates

In the quest of promising Indium free amorphous transparent conducting oxide (TCO), Zn-doped SnO₂/Ag/Zn-doped SnO₂ (OMO) multilayer films were prepared on flexible polyethylene terephthalate (PET) substrates by RF sputtering at room temperature (RT). Growth parameters were optimized by varying sputtering power and working pressure, to have high electrical conductivity and optical transmittance. Optimization of the thickness of each layer was done by Essential Macleod Program (EMP) simulation to get the higher transmission through OMO multilayer. The sheet resistance and transmittance of 3 at% Zn-doped SnO₂ thin film (30 nm) were 2.23 kΩ/□, (ρ ~ 8.92×10⁻³ Ω∙cm) and 81.3% (at λ ~ 550 nm), respectively. By using optimized thicknesses of Zn-doped SnO₂ (30 nm) and Ag (12 nm) and optimized growth condition Zn-doped SnO₂/Ag/Zn-doped SnO₂ multilayer thin films were deposited. The low sheet resistance of 7.2 Ω/□ and high optical transmittance of 85.1% in the 550 nm wavelength region was achieved with 72 nm multilayer film.     

Synthesis of KOH/SnO2 solid superbases for catalytic Knoevenagel condensation

KOH/SnO₂ solid superbases of specific morphology and uniform pore structure were synthesized. The SnO₂ support was prepared by reflux digestion using graphene oxide as template and employed for the loading of KOH by means of grinding and thermal treatment. With base strength of 26.5 ≤ H₋ < 33.0 and superbasic sites of 1.362 mmol g^− 1, the 20 wt.%KOH/SnO₂ catalyst exhibits excellent activity in Knoevenagel condensation under mild conditions. The catalytic efficiency is closely related to the base strength and the amount of superbasic sites. The findings disclose a new route for the synthesis of versatile solid superbases using SnO₂ as supports.     

Ultrafine SnO2 nanoparticles as a high performance anode material for lithium ion battery

In this paper, the ultrafine tin oxides (SnO₂) nanoparticles are fabricated by a facile microwave hydrothermal method with the mean size of only 14 nm. Phase compositions and microstructures of the as-prepared nanoparticles have been investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). It was found that the ultrafine SnO₂ nanoparticles are obtained to be the pure rutile-structural phase with the good dispersibility. Galvanostatic cycling and cyclic voltammetry results indicate that the first discharge capacity of the ultrafine SnO₂ electrode is 1196.63  mAh g⁻¹, and the reversible capacity could retain 272.63 mAh g⁻¹ at 100 mA g⁻¹ after 50 cycles for lithium ion batteries (LIBs). The excellent electrochemical performance of the SnO₂ anode for LIBs is attributed to its ultrafine nanostructure for providing active sites during lithium insertion/extraction processes. Pulverization and agglomeration of the active materials are effectively reduced by the microwave hydrothermal method.     

Mesoporous carbon nanofibers with large cage-like pores activated by tin dioxide and their use in supercapacitor and catalyst support

The mesoporous carbon nanofibers (MCFs) with large cage-like pores have been fabricated by thermally treating electrospun fibers of polyvinyl alcohol containing tin compound. During the process, tin oxide is reduced to melting tin and the carbon is activated to form the porous carbon. The results of X-ray diffraction and transmission electron microscopy at different temperatures show that particles of SnO₂ (∼1.9 nm) exist in the fibers at 300 °C while mixtures of Sn and SnO with rod-like shapes appear in the matrix when the fibers are heated at 400 °C, and that Sn migrates to the surface of fibers and pores are formed in the fibers at higher temperature. Specific surface area of MCFs can reach 800 m² g⁻¹ and the average diameter of interior pores is about 10.3 nm while the entrance pores are small. The specific capacitance of MCFs is 105 F g⁻¹ and the fabricated symmetrical capacitors exhibit high-rate capacitive properties and excellent stability, Pt nanoparticles which can be densely loaded on MCFs exhibit relatively high activity and stability toward electro-oxidation of methanol, which indicate that MCFs may be used as electrodes for high-rate energy storage and support for catalyst. This approach may be extended to prepare other porous carbon materials.     

Trimethylamine sensing properties of nano-SnO2 prepared using microwave heating method

The precursor was obtained through the reaction between SnCl₄·5H₂O and NaOH in the presence of PEG400 (polyethylene glycol, M = 400). Tin oxide (SnO₂) nano-powders were prepared by heating the precursor with microwave method. SnO₂ thick film sensors were fabricated using SnO₂ nano-materials as sensing materials. The phase composition and morphology of the material particles were characterized through X-ray diffraction (XRD) and transmission electron microscopy (TEM), respectively. The average particle sizes of the samples obtained with 616 W microwave heating and 800 W microwave heating (20 min) are about 5 and 15 nm, respectively. The influence of the heating duration and heating power on the gas-sensing properties of sensors based on SnO₂ nano-materials were investigated. The sensitivities of the sensors based on SnO₂ nano-materials heated with 616 and 800 W for 20 min were higher than those of the sensors based on SnO₂ nano-materials heated with 136, 264 and 440 W for 20 min. When operating at 200–310 °C, the sensor based on SnO₂ heated with 616 W for 20 min exhibits highest sensitivities in all sensors based on SnO₂ heated with 616 W for different duration. The sensitivity to a few kinds of organic gases, such as (CH₃)₃N and (CH₃)₂CO were studied. It was found that the sensor based on SnO₂ nano-materials (with 616 W microwave heating for 20 min) exhibited good performance characterized by high sensitivity and short response time to dilute trimethylamine when operated at 255 °C. The sensitivity to 0.001 ppm (CH₃)₃N at 255 °C was 3. The response time and recovery time were about 30 and 100 s, respectively.     

Electric field-assisted flash sintering of tin dioxide

SnO₂ green pellets were submitted to ac electric fields at temperatures below 1350 °C. Electric current pulses occurred and a substantial modification was found in the microstructure of the pellets after application of 80 V cm⁻¹ at 900, 1100 and 1300 °C. Similar experiments were carried out in SnO₂ mixed to 2 wt.% MnO₂. The linear shrinkage of the pellets was monitored with a dilatometer during the application of the electric field. Scanning electron microscopy micrographs of the pellets show the grain structure evolution after the electric current pulses. The larger is the electric current flow through the SnO₂ pellet, the larger are the shrinkage and the average grain size. Even though sintering occurs without significant densification in SnO₂, the welding of the grains is evident. The apparent density of green pellets of SnO₂ with MnO₂ addition sintered at 1100 °C increased 110% with the application of 80 V cm⁻¹, 5 A.     

Highly sensitive acetone sensor based on Eu-doped SnO2 electrospun nanofibers

In this study, a series of undoped and Eu-doped SnO₂ nanofibers were synthesized via a simple electrospinning technique and subsequent calcination treatment. Field-emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) were carefully used to characterize the morphologies, structures and chemical compositions of these samples. The results reveal that the as-prepared nanofibers are composed of crystallite grains with an average size of about 10 nm and Eu³⁺ ions are successfully doped into the SnO₂ lattice. Compared with pure SnO₂ nanofibers, Eu-doped SnO₂ nanofibers demonstrate significantly enhanced sensing characteristics (e.g., large response value, short response/recovery time and outstanding selectivity) toward acetone vapor, especially, the optimal sensor based on 2 mol% Eu-doped SnO₂ nanofibers shows the highest response (32.2 for 100 ppm), which is two times higher than that of the pure SnO₂ sensor at an operating temperature of 280 °C. In addition, the sensor exhibits a good sensitivity to acetone in sub-ppm concentrations and the detection limit could extend down to 0.3 ppm, making it a potential candidate for the breath diagnosis of diabetes.     

Raman spectra,photoluminescence and ferromagnetism of pure,Co and Fe doped SnO2 nanoparticles

The pure and transition metal (Co and Fe = 3 and 5 mol%) doped SnO₂ nanoparticles have been synthesized by a chemical route using polyvinyl alcohol as surfactant. These nanoparticles were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), Raman, Fourier transform infrared (FTIR) spectroscopy, photoluminescence (PL) and magnetic measurements. The XRD patterns show that all the samples have tetragonal rutile structure without any extra phase and the value of average particle size using FWHM lies within 12–29 nm is also confirmed by TEM. FTIR spectrum has been used to confirm the formation of SnO bond. Raman spectroscopy shows the intensity loss of classical cassiterite SnO₂ vibration lines which is an indication of significant structural modifications. From PL, an intense blue luminescence centered at a wavelength ～530 nm is observed in the prepared SnO₂ nanoparticles, which is different from the yellow-red light emission observed in SnO₂ nanostructures prepared by other methods. The strong blue luminescence from the as-grown SnO₂ nanoparticles is attributed to oxygen-related defects that have been introduced during the growth process. These Co and Fe-doped SnO₂ nanoparticles exhibit room temperature ferromagnetism and the value of their magnetic moment and phase transition temperature are sensitive to their size and stoichiometric ratio.     

Nanostructured SnO2 thin films for NO2 gas sensing applications

We report the synthesis of nanostructured SnO₂ by a simple inexpensive sol–gel spin coating method using m-cresol as a solvent. This method facilitates rapid synthesis at comparatively lower temperature enabling formation of nanostructures suitable for gas-sensing applications. Various physicochemical techniques have been used for the characterization of SnO₂ thin films. X-ray diffraction analysis confirmed the single-phase formation of tetragonal SnO₂ having crystallite size 5–10 nm. SnO₂ showed highest response (19%) with 77.90% stability toward 100 ppm nitrogen dioxide (NO₂) at 200 °C. The response time of 7 s and recovery time of 20 min were also observed with the same operating parameters. The probable mechanism is proposed to explain the selective response toward nitrogen dioxide. Impedance spectroscopy studies showed that the response to nitrogen dioxide is mainly contributed by grain boundaries. The reproducibility and stability study of SnO₂ sensor confirmed its candidature for detection of NO₂ gas at low concentration (10–100 ppm) and lower operating temperature.     

Synthesis,characterization and alcohol sensing property of Zn-doped SnO2 nanoparticles

The Zn-doped SnO₂ nanoparticles synthesized by the chemical co-precipitation route and having dopant concentration varying from 0 to 4 at%, were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM) for structural and morphological studies. XRD analyses reveal that all the samples are polycrystalline SnO₂ having tetragonal rutile structure with nanocrystallites in the range 10–25 nm. The TEM images show agglomeration of grains (cluster of primary crystallites). A corresponding selected area electron diffraction pattern reveals the different Debye rings of SnO₂, as analyzed in XRD. Alcohol sensing properties of all the Zn-doped samples were investigated for various concentrations of methanol, ethanol and propan-2-ol in air at different operating temperatures. Among all the samples examined, the 4 at% Zn-doped sample exhibits the best response to different alcohol vapors at the operating temperature of 250 °C. For a concentration of 50 ppm, the 4 at% Zn-doped sample shows the maximum response 85.6% to methanol, 87.5% to ethanol and 94.5% to propan-2-ol respectively at the operating temperature of 250 °C. A possible reaction mechanism of alcohol sensing has been proposed.     

Carbon-coated SnO2/graphene nanosheets as highly reversible anode materials for lithium ion batteries

A simple approach is reported to prepare carbon-coated SnO₂ nanoparticle–graphene nanosheets (Gr–SnO₂–C) as an anode material for lithium ion batteries. The material exhibits excellent electrochemical performance with high capacity and good cycling stability (757 mA h g^?1 after 150 cycles at 200 mA g^?1). The likely contributing factors to the outstanding charge/discharge performance of Gr–SnO₂–C could be related to the synergism between the excellent conductivity and large area of graphene, the nanosized particles of SnO₂, and the effects of the coating layer of carbon, which could alleviate the effects of volume changes, keep the structure stable, and increase the conductivity. This work suggests a strategy to prepare carbon-coated graphene–metal oxide which could be used to improve the electrochemical performance of lithium ion batteries.     

Tin–Zinc oxide composite ceramics for selective CO sensing

Composite metal oxide gas sensors were intensely studied over the past years having superior performance over their individual oxide components in detecting hazardous gases. A series of pellets with variable amounts of SnO₂ (0–50 mol%) was prepared using wet homogenization of the component oxides leading to the composite tin-zinc ceramic system formation. The annealing temperature was set to 1100 °C. The samples containing 2.5 mol% SnO₂ and 50 mol% SnO₂ were annealed also at 1300 °C, in order to observe/to investigate the influence of the sintering behaviour on CO detection. The sensor materials were morphologically characterized by scanning electron microscopy (SEM). The increase in the SnO₂ amount in the composite ceramic system leads to higher sample porosity and an improved sensitivity to CO. It was found that SnO₂ (50 mol%) - ZnO (50 mol%) sample exhibits excellent sensing response, at a working temperature of 500 °C, for 5 ppm of CO, with a fast response time of approximately 60 s and an average recovery time of 15 min. Sensor selectivity was tested using cross-response to CO, methane and propane. The results indicated that the SnO₂ (50 mol%)-ZnO (50 mol%) ceramic compound may be used for selective CO sensing applications.     

Carbon coated porous tin peroxide/carbon composite electrode for lithium-ion batteries with excellent electrochemical properties

A porous tin peroxide/carbon (SnO₂/C) composite electrode coated with an amorphous carbon layer is prepared using a facile method. In this electrode, spherical graphite particles act as supporter of electrode framework, and the interspace among particles is filled with porous amorphous carbon derived from decomposition of polyvinylidene fluoride and polyacrylonitrile. SnO₂ nanoparticles are uniformly embedded in the porous amorphous carbon matrix. The pores in amorphous carbon matrix are able to buffer the huge volume expansion of SnO₂ during charge/discharge cycling, and the carbon framework can prevent the SnO₂ particles from pulverization and re-aggregation. The carbon coating layer on the outermost surface of electrode can further prevent porous SnO₂/C electrode from contacting with electrolyte directly. As a result, the repeated formation of solid electrolyte interface is avoided and the cycling stability of electrode is improved. The obtained SnO₂/C electrode presents an initial coulombic efficiency of 77.3% and a reversible capacity of 742 mA h g⁻¹ after 130 cycles at a current density of 100 mA g⁻¹. Furthermore, a reversible capacity of 679 mA h g⁻¹ is obtained at 1 A g⁻¹.     

Effect of pyrolysis temperature on the pore structure evolution of polysiloxane-derived ceramics

Homogeneous silicon oxycarbide (SiOC) ceramic powders were prepared by pyrolysis of cross-linked polysiloxane at different temperatures (1250–1500 °C) under vacuum. The effect of pyrolysis temperature on the pore structure evolution was investigated by means of N₂ adsorption, SEM, XRD, IR and element analysis (EA). Studies showed that predominate mesoporous ceramics with the average pore size in the range of 2–13 nm were obtained after pyrolysis in this temperature range. The pore structure transformation is strongly correlated with the thermolytic decomposition process of the used precursor, such as phase separation and carbothermal reduction. At relatively lower temperature (1250–1350 °C), the ceramics had a relative small specific surface areas (35 m²/g) owing to the low degree of carbothermal reduction. However, as the carbothermal degree had an obvious augment at relative higher temperature (1400–1450 °C), the specific surface areas and total pore volume increased and reached to the maximum of 66 m²/g and 0.214 cm³/g, respectively, and subsequently decreased rapidly after 1500 °C for the reason of partial sintering of the nano-sized SiC derived from polysiloxane.     

Combustion synthesis and EIS characterization of TiO2–SnO2 system

TiO₂ is an insulator, but using specific dopants, can modify sharply its electronic structure towards semiconducting behavior. This type of response is widely applied in many electrochemical and electrocatalytical devices, namely chlorine production, hydrocarbon oxidation, CO and CO₂ hydrogenation and as electroactive substrata for biological cell growth.Combustion synthesis is a very simple, rapid and clean method for material preparation, which will be used in the preparation of the (1 − x)TiO₂–xSnO₂, x = 0.05–0.3. Tin oxalate and titanium isopropoxide are used as precursors for the synthesis. The as-prepared powders are fine and homogeneous, the average particle size is in the range of 5–10 nm, powders and ceramic compact bodies are characterized by DRX, SEM–TEM–EDX, DTA–TG and EIS. The impedance spectroscopy of the sample 10 mol% of SnO₂ indicates the presence of several phases which promote a matrix composite based in an electrical TiO₂ insulator compatible with an electronic conducting phase tin rich. This could be attributed to the spinodal decomposition effect observed in TiO₂–SnO₂ system.