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REVIEW 3 major objections 5 minor 62 references

On the Hidden Transient Interphase in Metal Anodes: Dynamic Precipitation Controls Electrochemical Interfaces in Batteries

T0 review · 3 major / 5 minor · reviewed 2026-08-12 · deepseek-v4-flash

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Pith's one-line read A transient salt skin that forms during fast discharge changes how metal anodes re-grow on the next charge.

desk verdict Worth a serious look: the transient salt film on dissolving Zn is real and well-evidenced, but the claim that it controls redeposition morphology needs a cleaner control experiment. read the letter →

arxiv 2411.16741 v3 pith:SFQ5ETML submitted 2024-11-23 cond-mat.mtrl-sci physics.chem-ph

Stephen T. Fuller , J.-X. Kent Zheng This is my paper · ORCID
classification cond-mat.mtrl-sciphysics.chem-ph
keywords transientsolid-electrolyteinterphasemetalanodezincdissolutionelectrodepositionsupersaturationsandequationrotatingdiskelectrodebattery
verification ladder T0 review T1 audit T2 compute T3 formal

The pith

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

The reading

The paper claims that a previously overlooked solid layer forms on metal anodes during fast discharge: when dissolution releases cations faster than they can diffuse away, the salt concentration at the surface exceeds saturation and a salt film precipitates. This Transient Solid-Electrolyte Interphase (T-SEI) passivates the electrode, self-limits dissolution, and leaves a flat, clean surface after it fully dissolves. The authors further claim that this brief event changes the next charging step: metal redeposited onto the relaxed surface grows by extending the original grains rather than forming new nuclei, reducing surface roughness by 42% in a proof-of-concept cycling test. The broader claim is that this dynamic precipitation—not only permanent, decomposition-derived SEI—governs electrochemical interfaces in concentrated and water-in-salt electrolytes.

What carries the argument

The central object is the Transient Solid-Electrolyte Interphase (T-SEI), a salt precipitate (e.g., ZnSO$_4$) formed at the electrode surface when the local cation concentration exceeds the salt solubility limit during fast dissolution. The modified Sand equation (eq. 2) governs its incubation time, relating the critical discharged capacity to the inverse current density; the interphase relaxes with a characteristic timescale $\tau_{R,SEI}$ once the current stops. It does the work of creating a self-limiting dissolution front and a clean, flat surface whose subsequent redeposition is epitaxial-like.

What would settle it

Run the same high-rate dissolution on a rotating-disk electrode at high rotation speed, which suppresses local supersaturation (and thus T-SEI) while maintaining high overpotential; then redeposit and check whether the deposit still shows compact grain growth, which would show the effect is not specific to T-SEI.

Watch

Extended reading notes

Core claim

In its own terms: fast electro-dissolution of a metal anode in concentrated electrolyte drives the local salt concentration past saturation, precipitating a salt-based interphase (T-SEI) that is distinct from classical SEI. The T-SEI forms almost instantly once supersaturation is reached (incubation time follows a modified Sand equation, $J\sqrt{t_{inc}} \propto (c_{sat} - c_{\infty})$), and dissolves completely within roughly 300 milliseconds of current removal. Its presence is marked by a voltage spike in chronopotentiometry, a sharp rise in charge-transfer resistance, and a drop in double-layer capacitance consistent with a thicker salt film. Once relaxed, the electrode is chemically cleaned and, on subsequent recharge, metal deposition proceeds by compact growth of existing coarse grains (~15–20 µm) rather than independent particulate nucleation, a regime that can be re-armed periodically by deliberate fast-discharge pulses.

Load-bearing premise

The causal claim that T-SEI formation, rather than the high current or overpotential itself, is responsible for the improved redeposition morphology is not isolated by a control experiment that suppresses T-SEI while keeping the high dissolution rate.

Editorial extensions

If this is right

  • Rapid discharge in concentrated electrolytes will routinely hit a T-SEI regime, so voltage spikes during battery cycling at high rates may be caused by transient salt precipitation rather than by classical ion-depletion effects.
  • A fully relaxed T-SEI surface changes the subsequent redeposition from independent nucleation to compact grain growth, which is a step toward flat, rechargeable metal anodes.
  • Because T-SEI relaxes on a sub-second timescale, ordinary post-mortem characterization will miss it; detecting it requires in-operando electroanalytical and optical methods with higher temporal resolution.
  • Periodic fast-discharge pulses can re-establish the T-SEI 'cleaning' effect, reducing surface roughness by 42% in a proof-of-concept symmetric-cell test, suggesting a practical protocol knob for battery management.
  • Any electrode process that produces cations at a high rate, such as fast cathode charging, is in principle susceptible to T-SEI formation, extending the relevance beyond metal anodes.

Reading between the lines

Editorial extensions of the paper, not claims the author makes directly.

  • Extension: the same supersaturation argument should apply to other cation-releasing interfaces, such as alkali-metal stripping in localized high-concentration electrolytes, where the solubility limit is closer to operating concentrations; the paper demonstrates the effect in zinc but does not test these cases.
  • Extension: the ~300 ms relaxation time implies that a practical diagnostic for T-SEI could be the linear $Q_c$ versus $J^{-1}$ signature and the accompanying voltage spike, which might be recognized in full-cell cycling data without special instrumentation.
  • Extension: the paper shows the improved morphology degrades at large capacities, so a natural follow-up is to test whether an optimal frequency and intensity of T-SEI pulses can sustain epitaxial growth over hundreds of cycles.
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Editorial analysis

A structured set of objections, weighed in public.

Desk editor's note, referee report, and a circularity audit.

Referee Report

3 major / 5 minor

Summary. The paper reports the discovery of a Transient Solid-Electrolyte Interphase (T-SEI) formed during fast anodic dissolution of Zn in concentrated ZnSO4 and ZnCl2 electrolytes. The authors argue that rapid dissolution produces local supersaturation, causing salt precipitation that passivates the electrode, leads to a self-limiting flat dissolution morphology, and fully dissolves upon rest. They further claim that, after relaxation, the T-SEI-modified surface promotes compact, grain-growth-dominated redeposition instead of the isolated particulate nucleation seen on pristine or low-rate-discharged electrodes. Evidence includes J-V deviations under stagnant vs. rotating conditions, constant-current chronopotentiometry voltage spikes and in-operando optical imaging, EIS showing increased charge-transfer resistance and decreased double-layer capacitance, post-mortem FIB-SEM/EDX showing no residual interphase, and SEM/EBSD/profilometry of dissolution and redeposition morphologies. The paper also derives a Sand-type relation Q_c ∝ J^-1 and demonstrates a proof-of-concept cycling protocol with periodic T-SEI formation.

Significance. If the central claim holds, the paper identifies a previously overlooked, purely transient passivating phase that controls both dissolution kinetics and the morphology of the subsequent plating step in concentrated battery electrolytes. The study's strength is its multi-modal approach: RDE voltammetry, chronopotentiometry, operando optical visualization, EIS, FIB-SEM/EDX, EBSD, and profilometry all point consistently toward the existence of a transient interfacial precipitate. The relaxation experiments and post-mortem absence of the interphase are particularly convincing for the transient character. The derivation of Eq. (3) is parameter-free in that it contains no fitted constants, and it yields a falsifiable linear relation; however, the predicted slope is not tested against measured transport properties. The main weakness is that the causal link between T-SEI formation and the improved redeposition morphology is not isolated from other consequences of high-rate anodic polarization, so the third pillar of the central claim is not yet fully established.

major comments (3)
  1. [Fig. 6 and 'Unusual morphological evolution promoted by T-SEI'] The central causal claim—that T-SEI formation, rather than the high-rate dissolution history itself, causes the subsequent compact, grain-growth redeposition—is not isolated in the reported experiments. In Fig. 6, the low-rate (0.1 V vs. Zn2+/Zn) and high-rate (5 V) discharge conditions differ in applied overpotential, current density, total charge time, and extent of anodic cleaning/electropolishing, so the observed differences in redeposition morphology could in principle be produced by the high dissolution current or overpotential alone. The paper's 'cleaning' argument based on reduced C/S/O EDX signals (Fig. 5D-F) is similarly consistent with high anodic polarization removing adventitious carbon. Because the RDE setup enables forced convection, a control experiment with high rotation during dissolution (suppressing supersaturation and T-SEI while retaining a high dissolution current/overpotential) would directly test the attribution; without such a control, the third pillar of the paper's central claim remains confounded. The paper's own observation that the compact-growth mode is not self-sustainable over cycling (Fig. S22) further indicates that the long-term benefit rests on the periodic-enforcement protocol, making the control experiment necessary rather than cosmetic.
  2. [Eqs. (1)-(3) and Fig. 3B] The linear Q_c-versus-J^-1 relation in Eq. (3) is a direct rearrangement of the modified Sand equation with no fitted parameter; consequently, the good linear fit in Fig. 3B does not by itself validate the T-SEI mechanism or the assumption that the voltage spike is set by saturation. The predicted slope, πD_i[(c_sat - c_infty)nF]^2/4, is not compared with independently measured diffusion coefficients and saturation concentrations, and the application of a binary, dilute-solution Sand equation to 3 M ZnSO4 is questionable given migration, non-ideal activity, and speciation in concentrated electrolytes. A quantitative test using literature or measured transport parameters, or a direct measurement of the precipitate composition, is needed to confirm that the spike corresponds specifically to salt precipitation rather than to another transport-limited process.
  3. [Fig. S23 and proof-of-concept cycling] The headline quantitative benefit—a 42% reduction in surface roughness—is reported without error bars, replicate numbers, or statistical analysis, and the proof-of-concept protocol differs from the control not only by the periodic potentiostatic 5 V stripping step but also by the sequence of stripping capacities and rest times. As presented, this result supports only a qualitative proof of concept, not the quantitative claim in the abstract. Please provide replicate statistics or soften the quantitative claim accordingly.
minor comments (5)
  1. [Equation numbering throughout] The number (4) is used twice, once for Laplace's equation in the text and once for the S_dr formula in Materials and Methods; please renumber to avoid ambiguity.
  2. [Figure 6 caption] The caption uses panel label 'I' twice, once for the redeposition SEM image and once for the EBSD image; the panel references in the text and caption should be aligned.
  3. [Main text, paragraph on relaxation times] The text refers to 'Table 2' for definitions of t_inc, t_inc,2, τ_R,SEI, and τ_R,conc, but no Table 2 appears in the manuscript body or in the captured supporting information; please include the table or move the definitions into the text.
  4. [Materials and Methods] In the electrolyte preparation paragraph, 'by weighting certain amounts of salts' should read 'by weighing', and the sentence 'the total counts from the resulting Zn peak were compared' has a subject-verb agreement issue.
  5. [Abstract and main text] The term 'T -SEI' is typeset with inconsistent spacing in several places; please use a consistent unspaced 'T-SEI' throughout the manuscript.

Circularity Check

0 steps flagged · score 0.0 of 10

No circularity: Sand-equation derivation is externally grounded, and the only notable weakness (missing convection control for the morphology claim) is a confound, not a circular reduction.

full rationale

The paper's central quantitative derivation—Eq. (2) and Eq. (3), Q_C = J t_inc = π D_i ((c_sat−c_i^∞) n F)^2 / (4 J)—is a direct rearrangement of the classical Sand equation with the saturation concentration difference replacing the bulk concentration. It introduces no fitted parameter and is not used to extract a constant that is then relabeled as a prediction; the linear Q_C vs J^−1 plot is a test of externally established transport theory against measured incubation times. The transient character of T-SEI is supported by independent measurements: rest-time-dependent t_inc,2 (Fig. S6), post-relaxation FIB-SEM absence (Fig. 5B-C), and RDE convection dependence (Fig. 2), none of which presuppose T-SEI existence by definition. Self-citations (refs. 27, 28) appear only as background/contrast for deposit morphology and Zn-anode relevance; no load-bearing premise rests on an author-overlapping citation. The weakest point is the causal attribution in Fig. 6: high-rate dissolution differs from low-rate dissolution in current, overpotential, and surface cleaning, and no forced-convection control suppresses T-SEI while retaining high overpotential. That is an experimental confound or missing-control issue, not a circular reduction where an output equals an input by construction. The 42% roughness claim also lacks replicate statistics, but under-determination is not circularity. Hence no circularity; score 0.

Assumptions & free parameters 0 free parameters · 5 assumptions · 1 invented entities

The paper introduces no explicit free parameters in its central derivation, which is a strength. However, the key assumptions (binary diffusion, precipitate composition, and causal attribution of the morphological effect) are not independently verified, and the quantitative model is not tested against literature values.

assumptions (5)
  • standard math Fick's second law and the classical Sand equation for binary electrolyte diffusion apply to the dissolution geometry.
    Invoked in Eq. (1)-(3) to derive the incubation time and critical capacity for T-SEI formation.
  • domain assumption Mass transport near the dissolving electrode can be described by a single equivalent binary diffusion coefficient D_i, neglecting migration and convection in the quiescent chronopotentiometry tests.
    Used in Eq. (2)-(3); no validation of this simplification for 3 M ZnSO4 or 30 m ZnCl2 is provided.
  • domain assumption The passivating layer that forms beyond the critical potential is precipitated ZnSO4 salt resulting from local supersaturation, not another solid phase.
    The paper infers the T-SEI composition from EIS and the absence of a residue after relaxation; no direct chemical identification of the precipitate is given.
  • domain assumption The T-SEI fully dissolves when the local concentration gradient relaxes to bulk, leaving no permanent interphase.
    Based on rest-interval experiments and FIB-SEM, but the dissolution kinetics of the precipitate are not directly measured.
  • domain assumption The subsequent compact, grain-coherent deposition morphology is caused by the T-SEI's cleaning effect rather than by the high dissolution overpotential or current density itself.
    Figure 6 compares low-rate vs high-rate discharge, but no control with high-rate dissolution under forced convection (which would suppress T-SEI) is performed, so the causal role of T-SEI is not isolated.
invented entities (1)
  • Transient Solid-Electrolyte Interphase (T-SEI) independent evidence
    purpose: Explains the transport-limited dissolution behavior, the voltage spike in chronopotentiometry, and the subsequent compact grain-growth deposition morphology.
    The existence of a transient salt precipitate is supported by in-operando optical imaging, EIS changes (increased R_ct, decreased C_dl), and the absence of a residue after relaxation. The model makes a falsifiable Q_c versus 1/J prediction, though the slope is not quantitatively validated against known constants.

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Cite this review

Pith. "Pith review of On the Hidden Transient Interphase in Metal Anodes: Dynamic Precipitation Controls Electrochemical Interfaces in Batteries." pith.science (2026). https://pith.science/paper/SFQ5ETML

@misc{pith2026241116741,
  author       = {Pith},
  title        = {Pith review of: On the Hidden Transient Interphase in Metal Anodes: Dynamic Precipitation Controls Electrochemical Interfaces in Batteries},
  year         = {2026},
  howpublished = {\url{https://pith.science/paper/SFQ5ETML}},
  note         = {Machine review of arXiv:2411.16741}
}
read the original abstract

The Solid-Electrolyte Interphase, SEI, formed on a battery electrode has been a central area of research for decades. This thin, complex layer profoundly impacts the electrochemical deposition morphology and stability of the metal in battery anodes. Departing from conventional approaches, we investigate metal dissolution, the reverse reaction of deposition, in battery environments using a state-of-the-art electroanalytical system combining a rotating-disk electrode and in-operando visualization. Our key finding is the presence of a Transient Solid-Electrolyte Interphase, T-SEI, that forms during fast discharging at high dissolution rates. We attribute T-SEI formation to transient local supersaturation and resultant electrolyte salt deposition. The T-SEI fundamentally alters the dissolution kinetics at the electrochemical interface, leading to a self-limiting morphological evolution and eventually yielding a flat, clean surface. Unlike a classical SEI formed due to electrolyte decomposition, the T-SEI is fully relaxable upon removal of the enforced dissolution current. The formation of T-SEI, surprisingly, plays a critical role in the subsequent electrodeposition. When the metal is redeposited on a fully relaxed T-SEI surface, the morphology is remarkably different from that deposited on pristine or low-rate discharged metal electrodes. Electron backscatter diffraction analysis suggests the deposition occurs via growth of the original grains. This is in stark contrast to the isolated, particulate nuclei seen on standard metal electrodes without T-SEI formation. Our findings provide important insights into the electrochemical kinetics at the metal-electrolyte interface, particularly in concentrated or water-in-salt electrolytes that are close to the salt saturation limit. The results suggest a new dimension for electrochemical engineering in batteries.

Figures

Figures reproduced from arXiv: 2411.16741 by the authors.

Figure 2
Figure 2. Understanding T-SEI formation dynamics using a Rotating Disk Electrode (RDE). Current density-voltage (𝐽-V) curves of electro-dissolution in (A) 20 mM, (B) 1 M, and (C) 3 M ZnSO4 aqueous electrolytes. Time-dependent current measured in constant-potential electro￾dissolution at different potentials with no rotation: (D) 1 M and (E) 3 M ZnSO4 aqueous electrolytes. The working electrode is Zn metal foil. Scan rate is 1… view at source ↗
Figure 3
Figure 3. Determination of the Critical Capacity Q [PITH_FULL_IMAGE:figures/full_fig_p003_3.png] view at source ↗
Figure 4
Figure 4. Probing T-SEI properties using Electrochemical Impedance Spectroscopy (EIS). (A)-(B) EIS data represented on a Nyquist plot at different dissolution potentials. (C) Fitted values of charge transfer resistance as a function of potential and (D) fitted values of double layer [PITH_FULL_IMAGE:figures/full_fig_p003_4.png] view at source ↗
Figures from the paper (2 more)
Figure 5
Figure 5. Figure 5: Surface characterization of the metal electrode after full [PITH_FULL_IMAGE:figures/full_fig_p004_5.png]
Figure 6
Figure 6. Figure 6: Influence of T-SEI formation on electrodeposition morphology. Scanning electron microscopy (SEM) images of (A)-(B) low rate discharged Zn electrodes at 0.1 V vs. Zn2+/Zn and (C)-(D) high-rate discharged Zn electrodes at 5 V vs. Zn2+/Zn after T-SEI formation and relaxat…

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Pith tools

Reviewed August 12, 2026 · model on record in the stance chip above.