Chia-Wei Hung

For commercial processes, through-hole AAO membranes are fabricated from high-purity aluminum by chemical etching. However, this method has the disadvantages of using heavy-metal solutions, creating large amounts of material waste, and leading to an irregular pore structure. Through-hole porous alumina membrane fabrication has been widely investigated due to applications in filters, nanomaterial synthesis, and surface-enhanced Raman scattering. There are several means to obtain freestanding through-hole AAO membranes, but a fast, low-cost, and repetitive process to create complete, high-quality membranes has not yet been established. Here, we propose a rapid and efficient method for the multi-detachment of an AAO membrane at room temperature by integrating the one-time potentiostatic (OTP) method and two-step electrochemical polishing. Economical commercial AA1050 was used instead of traditional high-cost high-purity aluminum for AAO membrane fabrication at 25 °C. The OTP method, which is a single-step process, was applied to achieve a high-quality membrane with unimodal pore distribution and diameters between 35 and 40 nm, maintaining a high consistency over five repetitions. To repeatedly detach the AAO membrane, two-step electrochemical polishing was developed to minimize damage on the AA1050 substrate caused by membrane separation. The mechanism for creating AAO membranes using the OTP method can be divided into three major components, including the Joule heating effect, the dissolution of the barrier layer, and stress effects. The stress is attributed to two factors: bubble formation and the difference in the coefficient of thermal expansion between the AAO membrane and the Al substrate. This highly efficient AAO membrane detachment method will facilitate the rapid production and applications of AAO films.

Anodic aluminum oxide (AAO) has been widely applied for the surface protection of electronic component packaging through a pore-sealing process, with the enhanced hardness value reaching around 400 Vickers hardness (HV). However, the traditional AAO fabrication at 0~10 °C for surface protection takes at least 3–6 h for the reaction or other complicated methods used for the pore-sealing process, including boiling-water sealing, oil sealing, or salt-compound sealing. With the increasing development of nanostructured AAO, there is a growing interest in improving hardness without pore sealing, in order to leverage the characteristics of porous AAO and surface protection properties simultaneously. Here, we investigate the effect of voltage on hardness under the same AAO thickness conditions in oxalic acid at room temperature from a normal level of 40 V to a high level of 100 V and found a positive correlation between surface hardness and voltage. The surface hardness values of AAO formed at 100 V reach about 423 HV without pore sealing in 30 min. By employing a hybrid pulse anodization (HPA) method, we are able to prevent the high-voltage burning effect and complete the anodization process at room temperature. The mechanism behind this can be explained by the porosity and photoluminescence (PL) intensity of AAO. For the same thickness of AAO from 40~100 V, increasing the anodizing voltage decreases both the porosity and PL intensity, indicating a reduction in pores, as well as anion and oxygen vacancy defects, due to rapid AAO growth. This reduction in defects in the AAO film leads to an increase in hardness, allowing us to significantly enhance AAO hardness without a pore-sealing process. This offers an effective hardness enhancement in AAO under economically feasible conditions for the application of hard coatings and protective films.

Humidity nanosensors play a vital role in modern technology industries, including weather forecasts, industrial manufacturing, agriculture, food and chemistry storage. In recent years, research on humidity sensors has focused on different materials such as ceramics, polymers, carbon-based materials, semiconductors, MXenes or triboelectric nanogenerators, each with their own advantages and disadvantages. Among them, anodic aluminum oxide (AAO) is a well-known ceramic humidity sensor material with a long history of research and development. AAO humidity sensors offer advantages such as simple manufacturing processes, controllable nanostructures, high thermal stability and biocompatibility. However, traditional AAO fabrication still has disadvantages like high costs and longer process times. Hence, finding a low-cost and efficient method to fabricate AAO for controlling different nanostructures to meet the requirements is consistently a major research topic. From our previous studies, we have studied the relationship between the AAO capacitive humidity sensor and its nanostructures. In this paper, we explore the effect of an AAO nanoporous structure controlled by an anodization voltage of 20–40 V on the resistive-type humidity sensor performance instead of a capacitive one. We efficiently apply one-step hybrid pulse anodization at 25 °C to significantly reduce the processing time compared to the traditional two-step process under 0–10 °C. The AAO nanostructures and their impact on sensor measurements of humidity at 20–80 RH% will be discussed in detail. An electrical resistive sensing mechanism is established for further performance improvement by controlling anodization voltage.

Nanoporous anodic aluminum oxide (AAO) is an important template for 1D nanomaterial synthesis. It is used as an etching template for nanopattern transfer in a variety of contexts, including nanostructured material synthesis, electrical sensors, optical sensors, photonic and electronic devices, photocatalysis, and hardness and anticorrosion improvement. In this review, we focus on various fabrication methods, pore geometry modification, and recent advances of AAO, as well as sensor applications linked to our environment, daily life, and safety. Pore geometry is concerned with the material composition, applied voltage mold, electrolyte type, temperature, and anodizing time during the fabrication of AAOs and for adjusting their pore size and profile. The applied voltage can be divided into four types: direct current anodization (DCA), reverse pulse anodization, pulse anodization (PA), and hybrid pulse anodization (HPA). Conventional AAOs are fabricated using DCA and mild anodization (MA) at a relatively low temperature (−5~15 °C) to reduce the Joule heating effect. Moreover, the issues of costly high-purity aluminum and a long processing time can be improved using HPA to diminish the Joule heating effect at relatively high temperatures of 20–30 °C with cheap low-purity (≤99%) aluminum. The AAO-based sensors discussed here are primarily divided into electrical sensors and optical sensors; the performance of both sensors is affected by the sensing material and pore geometry. The electrical sensor is usually used for humidity or gas measurement applications and has a thin metal film on the surface as an electrode. On the contrary, the AAO optical sensor is a well-known sensor for detecting various substances with four kinds of mechanisms: interference, photoluminescence, surface plasma resonance, and surface-enhanced Raman scattering (SERS). Especially for SERS mechanisms, AAO can be used either as a solid support for coating metal nanoparticles or a template for depositing the metal content through the nanopores to form the nanodots or nanowires for detecting substances. High-performance sensors will play a crucial role in our living environments and promote our quality of life in the future.