RESUMO

A solvothermal synthesis of ultrasmall cerium oxide nanoparticles (USCeOxNPs) with an average size of 0.73 ± 0.07 nm using deep eutectic solvent (DES) as a stabilizing medium at a temperature of 90 ºC is reported. Transmission electron microscopy (TEM) and energy dispersive spectroscopy (EDS) were used to morphologically characterize the USCeOxNPs. These revealed approximately spherical shapes with emission lines characteristic of cerium. Selected area electron diffraction (SAED) was used to determine the crystalline structure of the cerium oxide nanoparticles (CeO2NPs), revealing the presence of crystalline cubic structures. The USCeOxNPs-DES/CB film was characterized by scanning electron microscopy (SEM), which demonstrated the spherical characteristic of CB with layers slightly covered by DES residues. DES was characterized by Fourier transform infrared (FT-IR) and nuclear magnetic resonance (NMR), indicating its formation through hydrogen bonds between the precursors. An electrochemical sensor for dopamine (DA) determination in biological fluids was developed using the USCeOxNPs together with carbon black (CB). An enhanced current response was observed on DA voltammetric determination, and this can be attributed to the USCeOxNPs. This sensor displayed linear responses for DA in the range 5.0 × 10-7 mol L-1 to 3.2 × 10-4 mol L-1, with a limit of detection of 80 nmol L-1. Besides detectability, excellent performances were verified for repeatability and anti-interference. The sensor based on USCeOxNPs synthesized in DES in a simpler and environmentally friendly way was successfully applied to determine DA in biological matrix.

Assuntos

Cério , Dopamina , Técnicas Eletroquímicas , Cério/química , Dopamina/análise , Dopamina/sangue , Técnicas Eletroquímicas/métodos , Humanos , Solventes Eutéticos Profundos/química , Nanopartículas/química , Limite de Detecção , Nanopartículas Metálicas/química , Tamanho da Partícula

RESUMO

Despite the structural and electrochemical advantages of LiFePO4 (LFP) as a cathode material, the solid-state reaction commonly used as a method to produce it at the industrial level has known disadvantages associated with high energy and fossil fuel consumption. On the other hand, solution-based synthesis methods present a more efficient way to produce LFP and have advantages such as controlled crystal growth, homogeneous morphology, and better control of pollutant emissions because the reaction occurs within a closed system. From an environmental point of view, different impacts associated with each synthesis method have not been studied extensively. The use of less polluting precursors during synthesis, as well as efficient use of energy and water, can provide new insights into the advantages of each cathode material for more environmentally friendly batteries. In this work, a solvothermal method is compared to a solid-state synthesis method commonly used to elaborate LFPs at the commercial level in order to evaluate differences in the environmental impacts of both processes. The solvothermal method used was developed considering the reutilization of solvent, water reflux, and a low thermal treatment to reduce pollutant emissions. As a result, a single high crystallinity olivine phase LFP was successfully synthesized. The use of ethylene glycol (EG) as a reaction medium enabled the formation of crystalline LFP at a low temperature (600 °C) with a nano-plate-like shape. The developed synthesis method was evaluated using life cycle analysis (LCA) to compare its environmental impact against the conventional production method. LCA demonstrated that the alternative green synthesis process represents 60% and 45% of the Resource Depletion impact category (water and fossil fuels, respectively) of the conventional method. At the same time, in the Climate change and Particular matter impact categories, the values correspond to 49 and 38% of the conventional method, respectively.