Pilar Hidalgo

Surface segregation of additives on SnO2 based powders and their relationship with macroscopic properties

Abstract Surface properties of ceramic powders frequently play an important role in producing high-quality, high-performance, and reliable ceramic products. These properties are related to the surface bond types and interactions with the surroundings. Oxide surfaces generally contain adsorbed hydroxyl groups and modifications in the chemical composition of the surface may be studied by infrared spectroscopy. In this work, we prepared SnO2 containing Fe or Mg ions by organic chemical route derived from Pechini’s method. The prepared powders were characterized by infrared spectroscopy (FT-IR), X-ray diffraction (XRD), dynamic electrophoretic mobility and surface area determination. Results demonstrated that the studied additives segregate onto the oxide surface and modify the hydroxyl IR bands of the adsorbed hydroxyl groups. These surface modifications change some macroscopic properties of the powder such as the isoelectric point (IEP) in aqueous suspensions and the final specific surface area. The increase of the surface area with additive concentration is supposedly due to the reduction of surface energy of the powders when additives segregate on the powder surface.

Flow injection analysis of ethyl xanthate by gas diffusion and UV detection as CS2 for process monitoring of sulfide ore flotation

A sensitive and robust analytical method for spectrophotometric determination of ethyl xanthate, CH(3)CH(2)OCS(2)(-) at trace concentrations in pulp solutions from froth flotation process is proposed. The analytical method is based on the decomposition of ethyl xanthate, EtX(-), with 2.0 mol L(-1) HCl generating ethanol and carbon disulfide, CS(2). A gas diffusion cell assures that only the volatile compounds diffuse through a PTFE membrane towards an acceptor stream of deionized water, thus avoiding the interferences of non-volatile compounds and suspended particles. The CS(2) is selectively detected by UV absorbance at 206 nm (epsilon=65,000 L mol(-1) cm(-1)). The measured absorbance is directly proportional to EtX(-) concentration present in the sample solutions. The Beers law is obeyed in a 1x10(-6) to 2x10(-4) mol L(-1) concentration range of ethyl xanthate in the pulp with an excellent correlation coefficient (r=0.999) and a detection limit of 3.1x10(-7) mol L(-1), corresponding to 38 microg L(-1). At flow rates of 200 microL min(-1) of the donor stream and 100 microL min(-1) of the acceptor channel a sampling rate of 15 injections per hour could be achieved with RSD<2.3% (n=10, 300 microL injections of 1x10(-5) mol L(-1) EtX(-)). Two practical applications demonstrate the versatility of the FIA method: (i) evaluation the free EtX(-) concentration during a laboratory study of the EtX(-) adsorption capacity on pulverized sulfide ore (pyrite) and (ii) monitoring of EtX(-) at different stages (from starting load to washing effluents) of a flotation pilot plant processing a Cu-Zn sulfide ore.

Determination of low concentrations of the flotation reagent ethyl xanthate by sampled DC polarography and flow injection with amperometric detection.

A polarographic DC(tast) method with the static mercury drop electrode, SMDE, was developed for determination of the flotation collector ethyl xanthate (EtX) in the concentration range from 1x10(-5) to 8x10(-5) M. The potentiality of the method was demonstrated by evaluating the capacity of powdered galena ore (PbS) to adsorb EtX in a titration-like procedure. Sulfide could be determined simultaneously with EtX because in NaOH electrolyte their anodic waves are well separated (E(1/2) congruent with-0.72 and -0.42 V versus Ag/AgCl, respectively). In addition, a new FIA method was developed by adapting a simple device to the tip of the glass capillary of a mercury electrode and doing amperometric detection at a fixed potential of -0.1 V, always in the DC(tast) mode. No oxygen removal was required. Reproducible results were obtained at a frequency of 72 injections per h, with automatic renewal of the SMDE every second. The calibration curve for freshly prepared EtX standards rendered a straight line from 5x10(-6) to 8x10(-5) M with correlation coefficient of 0.997, suitable for real applications in flotation processes and its effluents.

Flow injection analysis of ethyl xanthate by in-line dialysis and UV spectrophotometric detection

A simple and sensitive spectrophotometric flow method for determination of low concentrations of the flotation collector O-ethyldithiocarbonate (ethyl xanthate, CH(3)CH(2)-O-CS(2)(-)) in solutions is described. The method is based on ethyl xanthate detection at 301nm in medium of NaOH 50mmolL(-1). By injection of 200muL of sample, the analytical method shows linear response for the ethyl xanthate concentration from 0.5 up to 500mumolL(-1). Successive injections of 4mumolL(-1) ethyl xanthate (n=23) show a coefficient of variation lower than 0.6%, denoting high repeatability. The detection limit is 0.3mumolL(-1). At a flow rate of 2.0mLmin(-1), a frequency of 120injections/h of ethyl xanthate can be attained. By introduction of a tangential dialysis cell in the FIA system, the manual sample filtration step with 0.22mum filter was eliminated and the residual interference of suspended material, was completely overcome even for unfiltered sludge suspension samples, an important advantage that compensates for the frequency reduction to 25injections/h elevation and detection limit elevation to 2mumolL(-1), still outreaching for many applications. Potential applications of the method embrace the at line determination of ethyl xanthate in the ore processing industry, control of the concentration at its optimal level during the flotation process, as well as monitoring of residues in the effluents.

Reator de UV-Ozônio com lâmpada a vapor de mercúrio a alta pressão modificada para tratamento superficial de óxidos transparentes condutivos utilizados em dispositivos poliméricos eletroluminescentes

An UV-Ozone reactor was developed with an ignition tube extracted into HID mercury lamp used to irradiation on zinc oxide (ZnO) and fluorinated tin oxide (FTO) films for PLEDs devices. Different exposures times were used. In contact angle measurements revealed better results for ZnO and FTO by 15 and 5 min, respectively. In Diffuse Reflectance Infra-red Fourier Transformed (DRIFT) spectroscopy allowed the observation of water, hydrocarbon and carbon dioxide adsorbed on the untreated TCO surfaces. After the UV-Ozone treatment the contaminants were significantly reduced or eliminated and the PLEDs devices decreased threshold voltages in comparison with respectively untreated TCOs.

Assembly and characterization of ZnO nanoparticles for Grätzel's solar cells

This research aimed to build hybrid solar cells, based on Grätzel method. We used the Polyethylene Terephthalate (PET) polymer as a substrate containing a layer of Indium Tin Oxide (ITO). Films of ZnO nanoparticles (ZnO NPs) synthesized by Pechini Method, and four different dyes were tested: Congo Red (CR), Bromocresol Green (BG), Acridine Orange (AO) and a Ruthenium Complex (RC). ZnO NPs were analyzed by XRD, which generated peaks corresponding to hexagonal wurtzite crystalline structure. We also conducted analysis by UV–Vis. Spectroscopy and Transmission Electron Microscope (TEM). Rietveld analysis determined the crystal size of 115.23 ± 28.16 nm. The deposition of ZnO and dye thin films were made through spin-coating. The electrical properties of the formed films were characterized with Van der Pawn method. Efficiency in converting light in electricity under an OSRAM 20W light bulb was tested after the devices were built. The smaller sheet resistance results were obtained for material containing: PET/ITO/ZnO/CR and PET/ITO/ZnO/AO. As expected, the best open-circuit voltage (Voc) results reached were 64 and 73 mV to CR and AO, respectively. Therefore, the results demonstrated satisfactory interaction between the ZnO-Dye-Electrolyte layers. Copyright