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arxiv: 2604.19847 · v1 · submitted 2026-04-21 · ❄️ cond-mat.mtrl-sci · physics.app-ph· physics.chem-ph

Recognition: unknown

Organosilane-functionalized hydrothermal-derived coatings on titanium alloys for hydrophobization and corrosion protection

S. Rahimipour , B. Rafiei , E. Salahinejad
Authors on Pith no claims yet

Pith reviewed 2026-05-10 02:23 UTC · model grok-4.3

classification ❄️ cond-mat.mtrl-sci physics.app-phphysics.chem-ph
keywords titanium alloyhydrophobizationcorrosion protectionHDTMS coatingalkaline treatmentwater contact angleTi-6Al-4V
0
0 comments X

The pith

Alkaline roughening followed by HDTMS coating turns titanium alloy hydrophobic and improves its corrosion resistance in salt water.

A machine-rendered reading of the paper's core claim, the machinery that carries it, and where it could break.

The paper tests Ti-6Al-4V alloy surfaces that are first roughened in NaOH solutions of different strengths and then coated with hexadecyltrimethoxysilane (HDTMS). Alkaline treatment alone produces a hydrophilic surface that corrodes faster in NaCl solution. The added HDTMS layer reverses the wetting behavior to strong hydrophobicity and restores, then exceeds, the original corrosion resistance. The best result is a water contact angle near 147 degrees on the sample treated in 3 molar NaOH before coating. The authors conclude that the paired process suits titanium parts exposed to moisture.

Core claim

The central claim is that hydrothermal alkaline treatment of Ti-6Al-4V followed by HDTMS functionalization produces a hydrophobic surface whose water contact angle reaches about 147 degrees and whose corrosion rate in NaCl drops markedly below that of the untreated alloy, even though the alkaline step alone worsens corrosion performance.

What carries the argument

The HDTMS organosilane coating deposited on the NaOH-roughened titanium surface, which lowers surface energy and creates a water-repellent barrier.

If this is right

  • The 3 molar NaOH plus HDTMS sequence gives the highest measured water contact angle of about 147 degrees.
  • Alkaline roughening by itself lowers corrosion resistance in NaCl solution.
  • The HDTMS step reverses the corrosion loss and yields a net improvement.
  • The combined treatment is presented as viable for titanium alloys in moisture-exposed settings.

Where Pith is reading between the lines

These are editorial extensions of the paper, not claims the author makes directly.

  • The same roughening-plus-silane sequence could be tried on other titanium grades or on aluminum alloys where corrosion under humid conditions is a problem.
  • Optimal NaOH concentration may trade off roughness for coating adhesion, so intermediate strengths should be checked for long-term stability.
  • If the coating survives cyclic wetting and drying, it might also reduce biofouling or scaling on titanium medical or marine parts.

Load-bearing premise

The HDTMS layer stays attached and continues to repel water over time under real moisture and mechanical conditions, and the corrosion gain comes mainly from that water repellency rather than from unrelated surface changes.

What would settle it

A test showing that the 147-degree contact angle falls below 90 degrees and the corrosion current density rises back to or above the untreated-alloy value after weeks of immersion or abrasion would falsify the central claim.

Figures

Figures reproduced from arXiv: 2604.19847 by B. Rafiei, E. Salahinejad, S. Rahimipour.

Figure 1
Figure 1. Figure 1: Schematic illustration of the hydrophobization process used. [PITH_FULL_IMAGE:figures/full_fig_p018_1.png] view at source ↗
Figure 2
Figure 2. Figure 2: FESEM micrographs of Samples 1 (a), 3 (b), 5 (c) and 7 (d). [PITH_FULL_IMAGE:figures/full_fig_p019_2.png] view at source ↗
Figure 3
Figure 3. Figure 3: EDS profiles of Samples 1 (a), 3 (b), 5 (c) and 7 (d). [PITH_FULL_IMAGE:figures/full_fig_p020_3.png] view at source ↗
Figure 4
Figure 4. Figure 4: Macrographs of a water droplet on the surfaces of Samples 1 (a), 2 (b), 3 (c), 4 (d), [PITH_FULL_IMAGE:figures/full_fig_p022_4.png] view at source ↗
Figure 5
Figure 5. Figure 5: Amounts of the sessile water contact angles on the samples, in terms of “mean ± [PITH_FULL_IMAGE:figures/full_fig_p022_5.png] view at source ↗
Figure 6
Figure 6. Figure 6: Potentiodynamic polarization curves of the samples. [PITH_FULL_IMAGE:figures/full_fig_p022_6.png] view at source ↗
Figure 7
Figure 7. Figure 7: EIS Nyquist (a), Bode impedance (b) and Bode phase angle (c) plots of the samples [PITH_FULL_IMAGE:figures/full_fig_p023_7.png] view at source ↗
read the original abstract

This work focuses on the structure, wettability and corrosion behaviors of Ti-6Al-4V alloy after roughening treatments in different concentrations of NaOH aqueous solutions followed by low surface energy hexadecyltrimethoxysilane (HDTMS) coating. In this regard, scanning electron microscopy, contact angle measurements, potentiodynamic polarization and electrochemical impedance spectroscopy were used to characterize the samples. In contrast to hydrophilicity caused by the hydrothermal alkaline treatments, the subsequent HDTMS coating donated considerable hydrophobicity. Typically, the highest sessile water contact angle (about 147 deg) was obtained for the sample treated in 3 molar NaOH solution followed by the HDTMS coating. In addition, the alkaline treatment reduced the corrosion resistance of the surface in a NaCl aqueous solution; however, the HDTMS hydrophobization process improved it significantly. It is eventually concluded that the coupled use of alkaline treatment and HDTMS functionalization can be further considered for moisture-exposed applications of Ti-based alloys.

Editorial analysis

A structured set of objections, weighed in public.

Desk editor's note, referee report, simulated authors' rebuttal, and a circularity audit. Tearing a paper down is the easy half of reading it; the pith above is the substance, this is the friction.

Referee Report

3 major / 3 minor

Summary. The manuscript examines the impact of hydrothermal alkaline treatments in NaOH solutions of varying concentrations (including 3 M) on Ti-6Al-4V alloy surfaces, followed by hexadecyltrimethoxysilane (HDTMS) coating. Using SEM for morphology, sessile-drop contact angle for wettability, and potentiodynamic polarization plus EIS for corrosion in NaCl, it reports that alkaline treatment increases roughness and hydrophilicity while HDTMS imparts hydrophobicity (peak ~147° for 3 M NaOH + HDTMS) and restores/enhances corrosion resistance despite the alkaline step reducing it initially. The work concludes the combined approach merits consideration for moisture-exposed applications.

Significance. If the reported short-term hydrophobicity and corrosion improvements hold, the study demonstrates a simple, scalable two-step protocol for functionalizing titanium alloys that leverages hydrothermal roughening plus silane chemistry. This could be relevant for corrosion protection in humid environments. The consistent use of standard techniques (SEM, contact angle, polarization, EIS) supports reproducibility of the immediate observations and provides clear before/after comparisons.

major comments (3)
  1. [Abstract and Conclusion] Abstract and Conclusion: The forward claim that the treatment 'can be further considered for moisture-exposed applications' is load-bearing but rests only on initial sessile-drop angles and single-cycle polarization/EIS data. No long-term immersion, cyclic wetting, or post-exposure adhesion tests are reported to confirm that the HDTMS layer remains adherent and effective under prolonged moisture exposure, undermining attribution of sustained protection primarily to hydrophobization.
  2. [Results (corrosion subsection)] Results (corrosion subsection): Corrosion parameters (e.g., corrosion current density, impedance values) are presented as showing 'significant' improvement with HDTMS, yet no error bars, replicate counts, or statistical analysis are provided. This weakens the quantitative claim of improvement relative to the alkaline-only baseline.
  3. [Discussion] Discussion: The paper attributes the restored corrosion resistance to the HDTMS hydrophobization step, but lacks a control (e.g., roughened surface with a non-hydrophobic coating of similar thickness) to isolate the contribution of low surface energy versus other possible changes in surface chemistry or morphology from the alkaline treatment.
minor comments (3)
  1. [Abstract] Abstract: The contact angle is stated as 'about 147 deg' without indicating whether this is a maximum, mean value, or from how many measurements, and without standard deviation.
  2. [Experimental methods] Experimental methods: The HDTMS coating protocol (concentration, immersion time, curing conditions) should be stated with greater precision to enable exact replication.
  3. [Figures] Figures: SEM images and EIS plots would benefit from explicit scale bars, consistent labeling of all sample conditions, and inclusion of equivalent circuit fits if used for EIS analysis.

Simulated Author's Rebuttal

3 responses · 0 unresolved

We thank the referee for the thoughtful and constructive comments on our manuscript. We have addressed each major point below with point-by-point responses. Where the comments identify clear gaps, we have revised the text accordingly or acknowledged limitations while defending the scope of the current study.

read point-by-point responses

  1. Referee: [Abstract and Conclusion] The forward claim that the treatment 'can be further considered for moisture-exposed applications' is load-bearing but rests only on initial sessile-drop angles and single-cycle polarization/EIS data. No long-term immersion, cyclic wetting, or post-exposure adhesion tests are reported to confirm that the HDTMS layer remains adherent and effective under prolonged moisture exposure, undermining attribution of sustained protection primarily to hydrophobization.

    Authors: We agree that the manuscript reports only short-term characterization and that long-term durability under cyclic or prolonged exposure would provide stronger support for sustained performance in moisture-exposed applications. The current work focuses on demonstrating the immediate effects of the two-step process on wettability and corrosion behavior. In the revised manuscript, we have tempered the language in both the abstract and conclusion to state that the approach 'may merit consideration for further development in moisture-exposed applications, subject to long-term durability validation' rather than implying immediate suitability. This revision clarifies the scope without overstating the data. revision: partial

  2. Referee: [Results (corrosion subsection)] Corrosion parameters (e.g., corrosion current density, impedance values) are presented as showing 'significant' improvement with HDTMS, yet no error bars, replicate counts, or statistical analysis are provided. This weakens the quantitative claim of improvement relative to the alkaline-only baseline.

    Authors: We acknowledge that the absence of error bars and replicate statistics limits the strength of the quantitative claims. In the revised version, we have added error bars derived from triplicate independent measurements for all corrosion parameters (i_corr, E_corr, and impedance values) in the relevant figures and tables. We have also updated the methods section to specify that all electrochemical tests were performed in triplicate and included a brief note on the observed variability. This addresses the concern directly and strengthens the presentation of the data. revision: yes

  3. Referee: [Discussion] The paper attributes the restored corrosion resistance to the HDTMS hydrophobization step, but lacks a control (e.g., roughened surface with a non-hydrophobic coating of similar thickness) to isolate the contribution of low surface energy versus other possible changes in surface chemistry or morphology from the alkaline treatment.

    Authors: The experimental design already includes a direct comparison between the alkaline-treated (hydrophilic, reduced corrosion resistance) and alkaline + HDTMS (hydrophobic, restored corrosion resistance) surfaces, which isolates the net effect of adding the HDTMS layer. We recognize that an additional control using a non-hydrophobic coating of comparable thickness on the roughened surface would help separate the role of surface energy from other chemical or morphological changes. Such a control was not included in the original study. We have expanded the discussion section to explicitly note this limitation and suggest it as a direction for future work, while maintaining that the observed correlation between hydrophobization and improved corrosion metrics supports our attribution within the reported scope. revision: partial

Circularity Check

0 steps flagged

No circularity: purely experimental measurements with no derivations or self-referential predictions

full rationale

The paper is an experimental materials science study reporting direct physical measurements (SEM, sessile-drop contact angles, potentiodynamic polarization, EIS) on NaOH-treated and HDTMS-coated Ti-6Al-4V samples. No equations, fitted parameters, mathematical derivations, or predictions appear. Central results (e.g., 147° contact angle for 3 M NaOH + HDTMS, improved corrosion resistance) are obtained from independent lab measurements on prepared coupons, not from any model that reduces to its own inputs. Self-citations, if present, are not load-bearing for the reported data. The forward-looking application statement is an extrapolation, not a circular claim.

Axiom & Free-Parameter Ledger

0 free parameters · 2 axioms · 0 invented entities

The paper is experimental and draws on standard surface-science and electrochemistry assumptions without introducing new free parameters, invented entities, or ad-hoc axioms beyond routine characterization methods.

axioms (2)
  • domain assumption Sessile-drop contact-angle measurements accurately reflect macroscopic surface wettability.
    The paper uses this standard metric to claim hydrophobicity without additional validation of surface homogeneity.
  • domain assumption Potentiodynamic polarization and EIS in NaCl solution provide reliable comparative measures of corrosion resistance.
    These electrochemical techniques are invoked as direct evidence of improved protection after HDTMS coating.

pith-pipeline@v0.9.0 · 5495 in / 1512 out tokens · 43853 ms · 2026-05-10T02:23:27.807066+00:00 · methodology

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    work page doi:10.1016/j.porgcoat.2020.105594 2013