Abstract

Anodic porous alumina is a known material based on an old industry, yet with emerging applications in nanoscience and nanotechnology. This is promising, but the nanostructured alumina should be fabricated from inexpensive raw material. We fabricated porous alumina from commercial aluminum food plate in 0.4 M aqueous phosphoric acid, aiming to design an effective manufacturing protocol for the material used as nanoporous filler in dental restorative composites, an application demonstrated previously by our group. We identified the critical input parameters of anodization voltage, bath temperature and anodization time, and the main output parameters of pore diameter, pore spacing and oxide thickness. Scanning electron microscopy and grain analysis allowed us to assess the nanostructured material, and the statistical design of experiments was used to optimize its fabrication. We analyzed a preliminary dataset, designed a second dataset aimed at clarifying the correlations between input and output parameters, and ran a confirmation dataset. Anodization conditions close to 125 V, 20 °C, and 7 h were identified as the best for obtaining, in the shortest possible time, pore diameters and spacing of 100–150 nm and 150–275 nm respectively, and thickness of 6–8 µm, which are desirable for the selected application according to previously published results. Our analysis confirmed the linear dependence of pore size on anodization voltage and of thickness on anodization time. The importance of proper control on the experiment was highlighted, since batch effects emerge when the experimental conditions are not exactly reproduced.

Highlights

  • Anodic porous alumina (APA) is a nanostructured material obtained with good uniformity on large area scale by means of inexpensive manufacturing process of anodization [1,2]

  • The preliminary APA dataset available before the start of the present work was properly analyzed by means of scanning electron microscopy (SEM) imaging and subsequent image analysis, as described in the experimental section

  • Few works are available in the literature on the DoE analysis of nanoporous alumina fabricated by anodization

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Summary

Introduction

Anodic porous alumina (APA) is a nanostructured material obtained with good uniformity on large area scale (order of 10 cm × 10 cm, extendible to 1 m × 1 m) by means of inexpensive manufacturing process of anodization [1,2]. A great deal of work on chemical sensors and biosensors based on optical principles different from SERS has been carried out [22], including drug delivery application on possible biomedical devices [23,24,25]. This condition of having a wide-spread old-standing industry and know-how—that of Al anodization—at service for a nanostructured material with increasing understanding and emerging applications in nanotechnology, is promising. In order to open the way for applications of APA in—possibly disposable—devices and/or products with broad spread on the market, use of much inexpensive raw material should be adopted

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