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Due to its chemical and thermal inertness, refractoriness and accessible manufacturing technology, porous anodic aluminum oxide (PAAO) has found wide application in microelectronics and nanosensors. PAOA is characterized by a high degree of ordering: a small spread of pore diameters and a hexagonal-periodic arrangement of pores. By changing the technological parameters of anodic oxidation, it is possible to vary the size of pores and oxide cells of PAOA. It is possible to form porous aluminum oxide as both mesoporous (pore diameter from 2 to 50 nm) and microporous (pore diameter over 50 nm). In recent years, researchers have been attracted by the opportunity to study the optical properties of materials (analytes) deposited inside porous aluminum oxide in order to develop optical biosensors for diagnosing diseases at early stages, which allows for effective prediction, treatment and monitoring of their progress [3, 4]. Before introducing various analytes, it is necessary to obtain samples with reproducible geometric characteristics (length, pore diameter, porous cell diameter, porosity). The structural properties of porous aluminum oxide and the chemical composition of its surface can vary depending on the composition and concentration of the electrolyte in which it is formed, as well as the modes of its formation. Therefore, the aim of this work was to achieve control and reproducibility of the structural properties and chemical composition of PAOA