Tetragonal Cassiterite Structure Research Articles

Low temperature dielectric studies of aluminum doped tin oxide nanoparticles

This study presents a facile sol-gel route for synthesizing pristine and Al-doped SnO2 nanoparticles. The phase purity of the synthesized nanoparticles was confirmed by powder X-ray diffraction (PXRD), revealing a tetragonal cassiterite structure for all samples. The crystallite size, determined by using the Scherrer equation and Willamson-Hall plot, ranged from 9.66 nm to 25.75 nm and exhibited an increasing trend with increasing doping concentration. Raman spectroscopy further corroborated this structural identification. The incorporation of aluminum (Al) into the tin oxide matrix was validated by energy-dispersive X-ray spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS) analysis. UV–visible spectroscopy revealed a reduction in the bandgap from 3.6 eV to 3.2 eV upon Al doping, attributed to the decreasing lattice strain with increasing Al content and other underlying mechanisms. The dielectric properties, including dielectric constant, dielectric loss, and AC conductivity, were examined as a function of frequency and doping concentration within the temperature range of 100 K–400 K. These properties exhibited an increasing trend up to 6 % Al doping. Interestingly, the 8 % doped sample exhibited the lowest dielectric loss and the highest AC conductivity, making it a promising candidate for applications in high-frequency electronics, energy storage, and ferroelectric devices.

Transparent conducting SnO2 thin films synthesized by nebulized spray pyrolysis technique: Impact of Sb doping on the different physical properties

The impact of antimony (Sb) doping concentration on the different physical properties of transparent conducting tin oxide (SnO2) thin films synthesized through nebulized spray pyrolysis (NSP) method have been explored systematically. X-ray diffraction (XRD) results reveal the tetragonal cassiterite structure of single phase SnO2 and the decrement of crystallite size with rising Sb doping concentration. Uniform and compact surface morphology with continuous distribution of grains and reduction of grain size with increasing dopant amount are illustrated by scanning electron microscopy (SEM). The stoichiometry of SnO2 film with 2% Sb doping is confirmed by energy dispersive X-ray spectroscopy (EDS) study. The optical transmittance is more than 85% in the visible region for undoped film and enhanced in the near infrared (NIR) spectral region for all the films. The transparency is reduced and the optical band gap is found to increase from 3.69 eV to 3.90 eV upon Sb inclusion. The extinction coefficient, refractive index, dielectric constant, dissipation factor, volume energy loss function, surface energy loss function, optical conductivity and optical density of the films are determined and interpreted for different dopant concentrations. The photoluminescence (PL) spectrum demonstrates the enhancement of emission intensity with increasing Sb incorporation representing its suitability in the application of solid state lighting. The lowest resistivity of 6.435 × 10−4 Ω cm and the highest carrier concentration of 1.316 × 1021 cm−3 are achieved for the film with 8% Sb doping concentration. The mobility of the studied degenerated films is varied from 54.743 cm2/Vs for undoped films to 7.378 cm2/Vs for 8% Sb doped film and limited by ionized impurity scattering. The film deposited with 2% Sb doping level exhibits the highest figure of merit values in both visible and NIR wavelength region indicating its better role in optoelectronic applications.

Structural, morphological and opto-electrical properties of transparent conducting SnO2 thin films: Influence of Sb doping

ABSTRACT Pure and antimony doped tin oxide (Sb:SnO2) thin solid films were synthesised through a simple and low-cost nebulised spray pyrolysis (NSP) route. The influence of Sb doping on the different physical properties of these films was systematically investigated. The results of X-ray diffraction (XRD) study exhibited polycrystalline in nature of all films with tetragonal cassiterite structure of single phase SnO2. XRD analysis also revealed the reduction in crystallite size as well as the grain size observed in scanning electron microscopy (SEM) with Sb doping concentration. The average transmittance of all the films was greater than 73% at the visible wavelength region and the transparency was reduced by Sb inclusion. The direct optical band gap value was the lowest of 3.94 eV for pure SnO2 and enhanced by Sb doping level. The effects of Sb doping concentration on extinction coefficient, refractive index, dielectric constant, optical conductivity and optical density of the films were examined. Photoluminescence spectrum revealed a broad violet emission peak near 390 nm and Sb doping intensified the peak. Both the resistivity and sheet resistance were found to vary in the range of 1.61 × 10−3 Ω.cm to 3.92 × 10−4 Ω.cm and 32.73 Ω/□ to 134.41 Ω/□, respectively with the variation of Sb doping concentration. The highest mobility and carrier concentration were 54.74 cm2/Vs and 7.02 × 1021 cm−3 for undoped and 10% Sb doped films, respectively. However, the figure of merit was found to be maximum of 1.38 × 10−3 (Ω/cm2)−1 for 5% Sb doping concentration among the films.

Design and application of highly responsive and selective rGO-SnO2 nanocomposites for NO2 monitoring

In this work, the reduced graphene oxide (rGO) was introduced into SnO2 nanospheres to form the rGO-SnO2 nanocomposites, which were used for designing a high-performance NO2 gas sensor. The rGO-SnO2 nanocomposites were synthesized by a simple hydrothermal method, with the GO consumption from 0.1 wt% to 0.6 wt%. The synthesized samples were characterized by XRD, SEM, AFM, TEM, FTIR, and XPS. Microstructural characterization indicates that both pure SnO2 and SnO2 nanospheres in rGO-SnO2 nanocomposites have a tetragonal cassiterite structure. Pure SnO2 is a series of microspheres with the diameter of 1–2 μm assembled by a lot of nanoplates. While the SnO2 nanospheres with the diameter of 40–60 nm uniformly distribute on the rGO sheets. The pure rGO based sensor, pure SnO2 based sensor and rGO-SnO2 nanocomposite based sensor were investigated in their gas sensing performance at the operating temperature of 75–175 °C. The 0.2 wt% rGO-SnO2 nanocomposites show a higher response of 53.57 and faster response/recovery time of 16 s/63 s to 3 ppm NO2 at 125 °C than pure rGO and pure SnO2. The test results indicate that the introduction of rGO into SnO2 improves its sensing performance. Moreover, the rGO-SnO2 nanocomposites exhibit a high selectivity and good reproducibility to NO2.

Influence of defect related oxygen vacancies in tuning the CO2 sensing properties of microwave treated SnO2 thin films

In this work, SnO2 based precursor sol is subjected to microwave irradiation for different duration before it is sprayed on to a pre heated substrate to form nanostructured thinfilm. The structural characterization of the prepared samples via X-ray diffraction (XRD) shows the formation of consistent films with tetragonal cassiterite structure. The crystallite size and microstructure exhibit remarkable variation upon high energy irradiation. The improvement in the carbon dioxide sensing property of the prepared samples is analysed with Keithley 2400 source meter.The mechanism of gas sensing has been explained via a series of characterization techniques including Field emission scanning electron microscopy (FESEM), Photoluminescence and Raman spectroscopy. The studies confirm that microwave assisted preparation technique helps to modify the gas-sensing properties by tuning the amount of defect related oxygen vacancies.

Effect of microwave irradiation on the gas sensing properties of SnO2 thin films

Several studies clearly show that the gas sensing activity of metal oxides especially SnO2 is governed by the nature of surfaces exposed to ambient gas. Consequently, control over film morphology, the size and shape of faces in crystallites, defects etc. are required for the development of better chemical gas sensors with increased sensitivity and selectivity. In the formation of nanoparticles, homogenous fast heating is desired and thereupon microwaves exposure is looked upon as supportive to play a fabulous role in the growth and structure of materials. In this work, microwave treated (0.5–4 min.) SnO2 based precursor sol is used to prepare nanoparticulate thin film by spray pyrolysis, and the morphology, as well as the grain characteristics, are modified to enrich the surface physico-chemical, electrical transport and gas sensing properties. The structural characterization via XRD shows the formation of consistent films with tetragonal cassiterite structure accompanied with some local defects. The crystallite size lies in the nano regime (28–36 nm). The texture coefficient of prominent planes shows marked variation upon energy irradiation. The improvement in the gas sensing properties of as prepared films is investigated. The film made from 1 min. irradiated precursor sol shows LPG response of 98.5% and the mechanism of gas sensing has been explained on the basis of structural investigations and morphological aspects. Field Emission Scanning Electron Micrograph (FESEM) and UV characterization confirm that microwave assisted preparation technique helps to modify the gas-sensing properties by tuning the amount of surface defects which is an overriding factor in the gas-sensing process and influences the gas molecule adsorption and catalytic reaction at the surface.

Effects of thermal treatment and layers’ number on SnO2 thin films properties prepared by sol-gel technique

Tin oxide layers are very important in photovoltaic applications. This paper presents an in-depth study of the SnO2 thin films deposited by the gel dip coating technique on glass substrates. The heat treatment and the number of layers effect on structural, morphological, optical and electrical properties were studied. Differential scanning calorimetry (DSC) and thermo-gravimetric analysis (TGA) showed that SnO2 crystallized at 402.5 °C. The diffraction spectra x-rays revealed that a formation of tetragonal cassiterite structure with a preferred growth orientation according to (101) plane. Exceptional film prepared at 200 °C preheated temperature is according to the (110) plane growth orientation. The size of the crystallites is strongly influenced by the preheated temperature, annealing temperature and a number of layers. The AFM images show homogeneous surfaces for all samples except the film prepared at a preheated temperature of 200 °C. However, it becomes smoother by increasing the number of layers. UV-Visible spectroscopy has shown that greater transparency is found in the infrared and visible domains (75%–96%). For all films, the optical band gap energy varies randomly with the preheated temperature; conversely, it increases from 3.83 eV to 3.88 eV for three-layer and six-layer films respectively. The energy gap decreases for samples with more than 6 layers. The minimum resistivity values are 8.1 10–1 Ω cm determined by the four probe method for the sample preheated to 400 °C without annealing temperature.

Effect Of Fluorine Doping On The Structural, Optical And Electrical Properties Of Spin Coated Tin Oxide Thin Films For Solar Cells Application

Transparent conducting oxide (TCO) thin films are materials of significance for their applications in optoelectronics and sun powered cells. Fluorine-doped tin oxide (FTO) is an elective material in the advancement of TCO films. This paper reports the impact of fluorine doping on structural, optical and electrical properties of tin oxide thin films for solar cells application. The sol-gel was prepared from anhydrous stannous chloride, SnCl2 as an originator, 2-methoxyethanol as a solvent, di-ethanolamine as a preservative and ammonium fluoride as the dopant source. FTO precursor solution was formulated to obtain 0, 5, 10, 15 and 20 % doping concentration and deposited on glass substrates by means of spin coater at the rate of 2000 rpm for 40 seconds. After pre-heated at 200 oC, the samples were annealed at 600 oC for 2 h. The structural, optical and electrical characteristics of prepared films were characterized using X-ray diffraction (XRD) analysis, UV-visible spectroscopy and electrical measurement. X-ray diffraction (XRD) investigation of the films demonstrated that the films were polycrystalline in nature with tetragonal-cassiterite structure with most extraordinary pinnacle having a grain size of 17.01 nm. Doping with fluorine decreases the crystallite size. There was increment in the absorbance of the film with increasing wavelength and the transmittance was basically reduced with increasing fluorine doping in the visible region. The energy band gaps were in the range of 4.106-4.121 eV. The sheet resistance were observed to decrease as the doping percentage of fluorine increased with exception at higher doping of 15 and 20 %. In view of these outcomes, FTO thin films prepared could have useful application in transparent conducting oxide electrode in solar cell.

Impact of aging on the structural, textural, and acid properties of WO3 - SO42− - SnO2 solid acids

Aging of solid acid catalysts (SAC) appears to be a hidden factor impacting the textural properties as well as the performance of catalysts. In this work, aged WO3-SO42--SnO2 catalysts were prepared via sol-gel method using two different percentage loadings of WO3 (15 wt% and 35 wt%) followed by three different calcination temperatures (CT) (200 °C, 400 °C, and 650 °C). The 24 h aging at both ambient temperature as well as 50 °C were performed on SO42--SnO2 hydrogel mixture prior to loading with an appropriate percentage of WO3 and then calcined. The catalysts were characterized by thermogravimetric analysis (TG–DTA), powder x-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), surface acidity, and N2 isothermal adsorption/desorption techniques. The structural and textural properties of the catalysts were compared with the previously prepared non-aged catalysts and found to be different. The catalysts calcined at 400 °C have poor crystalline structures whereas the 650 °C product has crystalline tetragonal cassiterite structure. The potentiometric titration with n-butylamine also indicated very strong acid sites for catalysts calcined at 400 °C but dependent on the aging method, and percentage loading of WO3. Generally, both the surface area and micro-pore volume decreased gradually with rising calcination temperature, whereas the total pore volume (VT) and a mean pore radius increased with rising CT.

Influence of Fe2+/Fe3+ ions in tuning the optical band gap of SnO2 nanoparticles synthesized by TSP method: Surface morphology, structural and optical studies

Fe doped nanostructured SnO2 thin films are prepared by a thermal spray pyrolysis (TSP) method at a substrate temperature (Ts) 450 °C. In addition, an effort is made to comprehend the effect of Fe doping on the surface morphology, micro-structural and optical properties of SnO2 thin film. The result of XRD data confirms that the fabricated SnO2 films are tetragonal cassiterite structure and the lattice parameters are slightly changed with Fe2+/Fe3+ contents. The values of lattice parameters are analogous in Rietveld refinement and DFT function. The lattice strain and stresses value are ranging from 2.07 to 0.13, × 10−3 and 0.71–0.04 respectively. The films are made up of nano-sized crystals with slender and polyhedron shaped particle size ranging from 17.23 to 159.50 nm observed by field emission scanning electron microscope (FESEM), Scherrer's formula and uniform deformation model (UDM). With increasing Fe concentrations, the optical band gap of SnO2 films is decreased from 3.89 to 3.39 eV. Reduction in optical band gap is attributed to the influence of Fe ions and conduction/valence bands of SnO2 structure. Fe doped SnO2 nanostructured film addresses the suitability of the material to have a good potential application in optoelectronic devices.

Effect of F and Nb co-doping on structural, electrical and optical properties of spray deposited tin oxide thin films

F and Nb co-doped tin oxide films were deposited from monobutyltin trichloride (C4H9SnCl3) on glass substrates at 470 °C by spray pyrolysis. The evolution of the film structure and morphology was investigated by X-ray diffraction and scanning electron microscopy, respectively. All the films were a single phase with polycrystalline, exhibiting a tetragonal cassiterite structure with (200) orientation. The introduction of F and Nb contributed to the growth of the films towards (200) crystal orientation and the formation of pyramidal shape particles with (101) twin planes. Resistivity, carrier concentration, and Hall mobility values of 3.62 × 10−4 Ω cm, 7.463 × 1020 cm−3, and 27.8 cm2 V−1 s−1, respectively, were achieved in the films for a dopant concentration of 20 at.% F and 1 at.% Nb in the precursor solution. Also, the transmittance of all the films in the visible range reached about 80% and the infrared reflectivity was oscillated between 92 and 96%.

Synthesis and characterization of organotin(IV) semicarbazones: potential precursors for nanosized tin oxide

A series of organotin(IV) semicarbazone adducts of the type R2SnCl2� nLH (1-6) were synthesized by the reactions of R2SnCl2 with newly synthesized car- vone semicarbazone (LH) in anhydrous ethanol (where R = CH3, n = 1( 1), 2 (2); R = C4H9, n = 1( 3), 2 (4); and R = C6H5, n = 1( 5), 2 (6)). All the compounds have been characterized by elemental analyses, FT-IR, NMR ( 1 H, 13 C, 119 Sn) and FAB mass spectral studies. 119 Sn NMR studies suggest monodentate mode of attachment of the ligand with central tin atom in the solution state. Thermogravimetric study of (6) shows large thermal events. Transformations of (4) and (6) to pure tin oxides (i and ii, respectively) have been carried out using sol-gel technique. Powder XRD patterns of the formed tin oxides indicate the formation of tetragonal cassiterite structure. SEM images of (i) and (ii) show wire- and grain-like morphologies of the crystallites, respectively. Graphical Abstract A series of organotin(IV) semicar- bazone adducts were synthesized by the reactions of diorganotin dichloride with newly synthesized carvone semicarbazone. Transformations of some of the newly synthesized adducts to pure tin oxides have been carried out using sol-gel technique. Powder XRD patterns of the formed tin oxides indicate the formation of tetragonal cassiterite structure, while SEM images show wire- and grain-like morphologies.

Sonochemical growth of SnO2 hollow nanostructures on cellulose acetate flexible substrates

In this paper, we report for the first time tin oxide hollow nanostructures growth on cellulose acetate flexible substrates by sonochemical spin coating. SnO2 particles formed by microwave irradiation of stannous chloride solution in ethylene glycol, used as starting material. Particles were then dissolved in ethanol and ultrasonicated just before ejecting from the spray jet to the substrates placed on the spin coater. The spin rate was maintained at 5000rpm and the process was repeated for several times. All the samples were annealed at 80°C for 2 to 6h and characterized by structural, morphological and optical studies. All the peaks in the X-ray diffractograms are identified and indexed as tetragonal cassiterite structure. AFM and SEM confirm the formation of porous tube- like growth in vertical direction. Strong photoluminescence peak in the visible region makes these structures suitable for flexible optoelectronic applications.

The effect of Mo and F double doping on structural, morphological, electrical and optical properties of spray deposited SnO2 thin films

The Mo/F double doped SnO2 films were successfully deposited via spray pyrolysis experimental technique. The effect of Mo/F co-doping on structural, morphological, electrical and optical properties of undoped SnO2 were investigated by means of XRD, SEM, four point probe and UV/VIS spectrophotometer measurements. The XRD measurements showed that films had a tetragonal cassiterite structure and the (211) preferential orientation of the undoped film changed to (301) and (200) orientations with high doping contents. Although the grain size values exhibited a decreasing tendency with increasing co-doping content, dislocation density and microstrain values of films usually had an increasing tendency. The SEM images indicated that the films were made up of well defined and homogenously dispersed pyramidal and polyhedron shaped nanoparticles. The electrical and optical studies showed the best electrical and optical properties were obtained for MFTO-2 sample. The best values of sheet resistance, optical band gap, figure of merit and IR reflectivity values were found to be 5.51Ω/□, 4.07eV, 1.67×10−2 (Ω/□)−1 and 97.13%, respectively. The observed results in the present study strongly suggest that the Mo/F double doped films are very appealing candidates for several technological applications.

Synthesis of SnO2 nanostructures by ultrasonic-assisted sol–gel method

Fluorine doped SnO2 nanostructures were grown using ultrasonic assisted sol–gel method. The gel was obtained by dissolving stannous chloride in methanol with ammonium fluoride as dopant followed by irradiation with ultrasonic vibrations. Obtained samples were characterized by structural, morphological and optical studies. All the peaks in the X-ray diffractograms are identified and indexed as tetragonal cassiterite structure. Negative slope of Williamson–Hall plots indicates compressive strain. Particle size of SnO2 nanostructures is decreases with increases in concentration of fluorine doping. Atomic force microscopy, scanning electron microscopy and transmission electron microscopy studies confirm the formation of ring like porous structures and then hollow tube like growth with increase in the fluorine concentration. Peaks in Raman spectra also indicate strong confinement in SnO2 particles. Distinct peaks in the PL spectra make the structure suitable for photovoltaic applications.

Effect of Sn precursor on the synthesis of SnO2 and Sb-doped SnO2 particles via polymeric precursor method

SnO2 and Sb-doped SnO2 particles were synthesized using the polymeric precursor method with different Sn salt precursors: SnCl2·2H2O, SnCl4·5H2O, or Sn citrate. Sb2O3 was used as the precursor of Sb, and the molar ratio of nSn:nSb was held constant. FTIR and TGA/DTA were used to examine the influence of the Sn precursor on the formation and thermal decomposition of the Sn and Sn-Sb complexes. The calcination products obtained from heating the Sn and Sn-Sb complexes at 500°C in air were analyzed using XRD and TEM analysis. The results revealed that the SnO2 and Sb-doped SnO2 formation temperatures depended on the nature of the Sn precursor. The calcination products were found to be SnO2 and Sb-doped SnO2 particles, which crystallized in a tetragonal cassiterite structure with a highly preferred (110) planar orientation. The Sn precursor and the presence of Sb in the SnO2 matrix strongly influenced the crystallinity and lattice parameters.

Characteristic evaluation on spray-deposited WFTO thin films as a function of W doping ratio

In this work, F and F + W simultaneously doped SnO2 highly transparent conducting thin films were deposited on glass substrates at (500 ± 5) °C temperature by the spray pyrolysis method. Microstructural, morphological, electrical and optical properties of FTO films were investigated as a function of tungsten (W) doping, in the range from 0 to 5 at%. X-ray diffraction patterns show that the films exhibit a tetragonal cassiterite structure and (200) preferential orientation of FTO film, and the relative strength of these peaks changes with altering the W doping ratio. The preferred growth of (211) changed to (200) plane with 2 at% W doping level and 3 at% W-doped film had (200) orientation and with further doping, this changed to (110) orientation. The scanning electron microscopy and atomic force microscopy images of the films indicate that the films are made up of dense small particles of a pyramidal shape and have a smooth surface. It was observed that the surface morphology of the films did not change much when the W element was inserted to the FTO structure. It was found that the sheet resistance values of the films varied with W doping ratio, and 2 at% W-doped FTO thin film exhibited the lowest values of sheet resistance (1.12 Ω). Also, the highest figure of merit, infrared reflectivity and optical band gap values were calculated for 2 at% W-doped FTO film as 50.9 × 10−2 Ω−1, 98.82 % and 4.13 eV, respectively. These results make the films an effective candidate for usage in many optoelectronic applications and photo-thermal conversion of solar energy.

An investigation of the Nb doping effect on structural, morphological, electrical and optical properties of spray deposited F doped SnO2 films

F and Nb + F co-doped SnO2 thin films were deposited on glass substrates by the spray pyrolysis method. The microstructural, morphological, electrical and optical properties of the 10 wt% F doped SnO2 (FTO) thin films were investigated specifically for niobium (Nb) doping in the range of 0–4 at.% with 1 at.% steps. As shown by the x-ray diffraction patterns, the films exhibited a tetragonal cassiterite structure with (200) preferential orientation. It was observed that grain sizes of the films for (200) and (301) peaks depended on the Nb doping concentration and varied in the range of 25.11–32.19 and 100.6–183.7 nm, respectively. The scanning electron microscope (SEM) micrographs showed that the FTO films were made of small pyramidal grains, while doubly doped films were made of small pyramidal grains and big polyhedron grains. From electrical studies, although 1 at.% Nb doped FTO films have the lowest sheet resistance and resistivity values, the highest figure-of-merit and optical band gap values obtained for FTO films were 16.2 × 10−2 Ω−1 and 4.21 eV, respectively. Also, infrared reflectivity values of the films were in the range of 97.39–98.98%. These results strongly suggest that these films are an attractive candidate for various optoelectronic applications and for photothermal conversion of solar energy.

Effect of Nb doping on structural, electrical and optical properties of spray deposited SnO2 thin films

Nb doped SnO2 transparent conducting thin films were deposited by spray pyrolysis method. Microstructural, morphological, electrical and optical properties of the films were investigated as a function of niobium (Nb) doping, in the range from 1.0% to 4.0% by atomic percent (with 1.0at.% step). From XRD patterns the films exhibited a tetragonal cassiterite structure. Although (211) peak is the most intense peak which is observed for all samples, the (301) reflection has the highest texture coefficient. The grain size values for (211) and (301) peaks were dependent on Nb doping concentration and they varied in the range of 34.99–24.15nm and 131.4–216.7nm, respectively. The SEM images of the films showed that the films were made up of grains with polyhedron like shape and that smaller grains were mostly seen in the spaces between polyhedron like grains. Also, SnO2 thin film doped with 2.0at.% Nb exhibited lowest values of sheet resistance (6.84Ω) and resistivity (0.62×10−3Ωcm), beside the highest value of figure of merit (3.4×10−3Ω−1) was obtained for 1.0at.% Nb doped thin film. The direct optical band gap decreased from 3.98eV to 3.73eV with increasing Nb concentration. These results make Nb doped SnO2 films an attractive candidate for many optoelectronic applications.

Structural and chemical characterization of SnO2-based nanoparticles as electrode material in Li-ion batteries

Improvement of long-term stability of electrode materials in Li-ion batteries requires a detailed understanding of influence of synthesis parameters on surface chemistry and on properties. Therefore, bare SnO2 and core/shell nanoparticles with SnO2 core and a hydrocarbon shell are synthesized in an Ar/20% O2 microwave plasma, deposited as porous nanoparticle films in situ on heated Ni-substrates, and finally assembled as anodes in Swagelok cells. In a comprehensive study, we investigate structure, particle size, chemistry, morphology, and water content of the nanoparticles using X-ray diffraction, transmission electron microscopy, specific surface area analysis, and coulometric water titration. The thicknesses of the nanoparticle films and their surface chemistry are investigated by scanning electron microscopy and X-ray photoelectron spectroscopy. SnO2 nanoparticles are crystalline, with a tetragonal cassiterite structure. Primary particle sizes around 3 nm are reached for the bare SnO2 particles, 5–8 nm for the cores of the core/shell nanoparticles. A minimum microwave power of 900 W is necessary to synthesize SnO2 nanoparticles without precursor residuals as pristine SnO2 particles for the subsequent coating step. In the coating step increasing hydrocarbon content can be correlated with increasing carbon-precursor feeding rate. Water uptake, stemming either from the process, or due to atmospheric contamination, can successfully be reduced by a thermal treatment. The still remaining water is a function of specific surface area. Finally, bare SnO2 versus core/shell nanoparticles are compared regarding the influence of the shell on the electrochemical properties. The principal improved functionality of the developed anodes in Swagelok cells is demonstrated.