Effect of Chemical Surface Texturing on the Superhydrophobic Behavior of Micro–Nano-Roughened AA6082 Surfaces
Abstract
:1. Introduction
2. Materials and Methods
2.1. Materials
2.2. Synthesis of Superhydrophobic Surfaces
- HNO3/HCl etching: The cleaned sample was dipped in a mixture of HNO3 and HCl in an ultra-pure water (1:3:3 ratio in vol.) solution for 60 min.
- HF/HCl etching: The aluminum specimens were dipped for 15 s in a HCl/HF acidic solution (73 vol.% HCl, 5 vol.% HF and 22 vol.% bi-distilled water).
- Boiling water treatment: Aluminum substrates were pretreated in boiling water for 5 min and dried at 70 °C for 60 min.
2.3. Sample Characterization
3. Results and Discussion
3.1. Surface Morphology
- HNO3/HCl etching: The surface was characterized by a bimodal structure. The coupled action of hydrochloric and nitric acids generated a micro-scale plate-like profile with numerous nano-scale pits (Figure 1a). This morphology is a result of the substrate interaction with this specific acidic solution. It is well known that aluminum alloys react strenuously with hydrochloric acid with a preferential attack of higher energy areas such as dislocations and grain boundaries, usually inducing large, rectangle-shaped pits [74]. However, due to the severe aggressiveness of the solution, the etched areas should be characterized by a non-homogeneous and uniform distribution and size (wider than 1 μm). In such a context, Oh et al. [75] suggested to not use only hydrochloric acid for aluminum etching but a mixture of acidic solution in order to reduce the dissolution rate on the local area and to obtain smaller pits. According to Singh et al. [76], oxidizing acids, such as nitric acid, have less effective corrosive actions on aluminum alloy. The combination of the hydrochloric and nitric acid action can be considered a successful approach to create a hierarchical structure as well as the micro-scale platelet structure that can be seen in the SEM image (Figure 1a).
- HF/HCl etching: The surface morphology of aluminum after the HF/HCl etching and the silane coating steps are shown in Figure 1b. A bimodal morphology can be clearly identified on the surface, i.e., a coral-like structure characterized by the presence of a pixelated substructure at the nanoscale level. In addition, in this case, the microstructure is a consequence of the intrinsic substrate heterogeneity. Indeed, the aluminum alloy has a large number of dislocations and line defects. These local defects are more reactive than other substrate areas in this acidic etchant [75]. Meanwhile, the impurities in the neighborhood of these defects could also magnify the chemical etching reaction. The dissolution phenomena in the aluminum induced by hydrofluoric acid starts after a relatively high immersion time (30–50 min) [77]. According to Straumanis et al. [77], the addition of a small quantity of hydrofluoric acid to other acids allows the electrochemical dissolution of the alloy to be promoted. In addition, HF acid reacts with Si-rich precipitates, favoring a selective dissolution in its neighboring area, thus influencing the large corrosion phenomena induced by a HCl acid solution. The selective dissolution favored by HF, coupled with the wide and general action of HCl, could be considered responsible for the coral-like structure obtained (Figure 1b).
- Boiling water treatment: An environmentally friendly and simple technique to obtain a nanostructured surface was applied. The absence of caustic reagents and special equipment in the whole preparation procedure make it industrially scalable and a cost-effective method. The SEM micrographs of the Al alloy surfaces treated with boiling water are shown in Figure 1c, before and after silanization. At the nano-scale level, the surfaces appeared to be covered by an oxi-hydroxide layer with 3D flower-like structures. This flower-like cluster consists of numerous petals with a thickness of ~30 nm. These contiguous petals overlap and connect to each other, resulting in a complex micro–nano structure. This microstructure is due to the formation of a protective film composed mainly of boehmite, according to the following reaction:
3.2. Profile Characterization
3.2.1. As-Received
3.2.2. HNO3/HCl Etching
3.2.3. HF/HCl Etching
3.2.4. Boiling Water Treatment
3.3. Roughness Statistical Analysis
3.4. Wettability
3.5. Self Cleaning Behavior
4. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Conflicts of Interest
Appendix A
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Samples | Step 1 | Step 2 |
---|---|---|
Al-R | – | – |
Al-RS | – | S18 |
Al-N | HNO3/HCl etching | – |
Al-NS | HNO3/HCl etching | S18 |
Al-F | HF/HCl etching | – |
Al-FS | HF/HCl etching | S18 |
Al-W | Boiling water | – |
Al-WS | Boiling water | S18 |
Sample | Arith. Roughness Ra (Sa) (nm) | Rms Roughness (Sq) (nm) | Skewness, S | Kurtosis, K |
---|---|---|---|---|
Al-R | 10.7 | 16.3 | 0.13 | 3.27 |
Al-N | 33.1 | 43.1 | 0.08 | 0.80 |
Al-NS | 14.9 | 21.7 | 0.03 | 2.19 |
Al-W | 27.5 | 36.4 | 0.17 | 1.41 |
Al-WS | 30.8 | 37.4 | −0.13 | 0.04 |
Al-F | 181.0 | 229. | 1.34 | 2.01 |
Al-FS | 138.0 | 169.8 | −0.51 | 0.18 |
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Khaskhoussi, A.; Calabrese, L.; Patané, S.; Proverbio, E. Effect of Chemical Surface Texturing on the Superhydrophobic Behavior of Micro–Nano-Roughened AA6082 Surfaces. Materials 2021, 14, 7161. https://doi.org/10.3390/ma14237161
Khaskhoussi A, Calabrese L, Patané S, Proverbio E. Effect of Chemical Surface Texturing on the Superhydrophobic Behavior of Micro–Nano-Roughened AA6082 Surfaces. Materials. 2021; 14(23):7161. https://doi.org/10.3390/ma14237161
Chicago/Turabian StyleKhaskhoussi, Amani, Luigi Calabrese, Salvatore Patané, and Edoardo Proverbio. 2021. "Effect of Chemical Surface Texturing on the Superhydrophobic Behavior of Micro–Nano-Roughened AA6082 Surfaces" Materials 14, no. 23: 7161. https://doi.org/10.3390/ma14237161