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arxiv: 2604.12670 · v1 · submitted 2026-04-14 · ❄️ cond-mat.mtrl-sci

Role of diffusion-induced grain boundary migration during molten salt corrosion of a Ni-30Cr alloy

Konnor Walter , Jagadeesh Sure , Adrien Couet , Emmanuelle A. Marquis This is my paper

Pith reviewed 2026-05-10 15:23 UTC · model grok-4.3

classification ❄️ cond-mat.mtrl-sci
keywords diffusion-induced grain boundary migrationmolten salt corrosionNi-30Cr alloydealloyingchromium depletionmicrostructureporous layer
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The pith

Diffusion-induced grain boundary migration drives chromium loss beyond lattice diffusion limits in Ni-30Cr molten salt corrosion.

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

The paper compares electropolished and sanded surfaces of a Ni-30Cr alloy exposed to LiCl-KCl-2wt% EuCl3 at 500 °C for 96 hours. On electropolished surfaces, dissolution proceeds slowly layer by layer over grain interiors, limited by nickel dissolution kinetics, while grain boundaries undergo DIGM to form isolated nickel islands. Sanded surfaces, after recrystallization, develop dense grain boundaries that migrate via DIGM, producing several micrometers of interconnected porosity with complete chromium depletion. This establishes DIGM as the mechanism responsible for long-range solute loss and shows that the alloy's near-surface grain structure decides the severity of attack. A reader would care because the result points to microstructure as a controllable variable for limiting corrosion in molten-salt environments.

Core claim

In the absence of fast diffusion pathways, dissolution occurred layer by layer and was kinetically controlled by Ni dissolution, as observed over the grain interiors of the electropolished sample. Grain boundaries were subject to diffusion-induced grain boundary migration (DIGM), leading to the formation of pure Ni islands above grain boundaries. This overall behavior contrasted with the sanded surface response that was characterized by several micrometer deep interconnected porosity and complete Cr depletion. DIGM of the dense grain boundaries created by recrystallization of the sanded surface was responsible for the observed sub-surface microstructure.

What carries the argument

Diffusion-induced grain boundary migration (DIGM), the motion of grain boundaries driven by solute diffusion that sweeps through the alloy, rapidly transports chromium outward and creates new nickel-rich structures.

If this is right

  • Corrosion remains shallow and layer-limited when grain-boundary density is low, as seen on electropolished surfaces.
  • Surface recrystallization activates extensive DIGM and produces deep, interconnected porosity.
  • Kinetics inside unaffected grains are set by nickel dissolution rather than chromium diffusion rates.
  • Alloy corrosion response in molten salts can be altered by changing initial grain-boundary density or character.

Where Pith is reading between the lines

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

  • Alloys or processing routes that pin grain boundaries or suppress recrystallization could reduce DIGM-driven attack without changing bulk composition.
  • The same boundary-migration process may operate in other dealloying or selective-dissolution systems, offering a general transport mechanism.
  • Systematic variation of annealing temperature before exposure would separate recrystallization effects from mechanical damage introduced by sanding.
  • In engineering components, fabrication steps that set near-surface grain structure could determine long-term performance under sustained molten-salt contact.

Load-bearing premise

The stark difference in corrosion depth and morphology between electropolished and sanded surfaces arises solely from DIGM enabled by recrystallization-induced grain boundary density, rather than from other unmeasured effects of sanding such as residual stress, surface contamination, or altered oxide layers.

What would settle it

In-situ microscopy that tracks whether grain boundaries migrate only on the sanded surface and whether that migration spatially correlates with the depth of porous chromium depletion would confirm the claim; deep porosity forming without observable boundary motion would falsify it.

Figures

Figures reproduced from arXiv: 2604.12670 by Adrien Couet, Emmanuelle A. Marquis, Jagadeesh Sure, Konnor Walter.

Figure 1
Figure 1. Figure 1: Average concentrations (measured by ICP-MS) of dissolved Ni and Cr metal ions in the post-corrosion salts. SEM images of the surfaces before corrosion are provided in [PITH_FULL_IMAGE:figures/full_fig_p007_1.png] view at source ↗
Figure 3
Figure 3. Figure 3: Surface SEM images (secondary electrons) of the EP surface (top) and the sanded surface (bottom) after removal of the salt. (a, e) low magnification images of EP and sanded surfaces (b) Higher magnification image from the EP surface shown the different surface b ) a) [PITH_FULL_IMAGE:figures/full_fig_p008_3.png] view at source ↗
Figure 4
Figure 4. Figure 4: SEM images (secondary electron) and SEM-EDS maps taken from the EP (top) and sanded (bottom) surface after removal of the salt with corresponding EDS elemental maps for (b, e) Cr and (c, f) Ni. STEM observations of cross-sections were conducted to better understand the structure and chemistry of the surface and subsurface for each sample condition. For the EP sample ( [PITH_FULL_IMAGE:figures/full_fig_p00… view at source ↗
Figure 5
Figure 5. Figure 5: (a) STEM image (HAADF) of a cross-section from the corrosion tested EP Ni-30Cr sample containing a grain boundary. (b) Corresponding EDS elemental map. (c) Cr composition profiles of the lines 1 and 2 indicated in (b), respectively. For the sanded sample, a very different microstructure was observed. First, the presence of Cr on the surface of the dark regions was attributed to a local thin Cr-rich oxide l… view at source ↗
Figure 6
Figure 6. Figure 6: FIB cross-section from the dark region of the corrosion-tested sanded surface of the Ni-30Cr alloy, with corresponding EDS elemental maps for (b) Cr and (c) Ni [PITH_FULL_IMAGE:figures/full_fig_p011_6.png] view at source ↗
Figure 9
Figure 9. Figure 9: Cross-section SEM images (secondary electron) of (a) the sanded surface before corrosion exposure, and (b) after thermal annealing at 500 °C for 96 hours (without corrosion exposure). Because the present results demonstrate that surface deformation triggers DIGM-assisted dealloying and results in a bi-continuous structure, previously reported corrosion morphologies may be reinterpreted through this lens. I… view at source ↗
read the original abstract

The response of Ni-Cr alloys to exposure to molten chloride and fluoride salts is typically characterized by Cr dealloying with the formation of a Cr-depleted bi-continuous porous subsurface layer. The exact mechanism behind the loss of Cr over distances unattainable by lattice diffusion alone is still debated. To address this question, two different surface finishes, namely electropolished and sanded, of a Ni-30Cr alloy were exposed to LiCl-KCl-2wt% EuCl3 eutectic salt at 500 {\deg}C for 96 hours. In the absence of fast diffusion pathways, dissolution occurred layer by layer and was kinetically controlled by Ni dissolution, as observed over the grain interiors of the electropolished sample. Grain boundaries were subject to diffusion-induced grain boundary migration (DIGM), leading to the formation of pure Ni islands above grain boundaries. This overall behavior contrasted with the sanded surface response that was characterized by several micrometer deep interconnected porosity and complete Cr depletion. DIGM of the dense grain boundaries created by recrystallization of the sanded surface was responsible for the observed sub-surface microstructure. This work unequivocally establishes DIGM as a key mechanism in alloy molten salt corrosion, and microstructure as a decisive contributor to an alloy's corrosion response.

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

2 major / 1 minor

Summary. The manuscript examines the mechanism of Cr dealloying in a Ni-30Cr alloy during exposure to LiCl-KCl-2wt% EuCl3 molten salt at 500°C for 96 h by contrasting electropolished and sanded surface finishes. On electropolished surfaces, dissolution proceeds layer-by-layer in grain interiors while grain boundaries undergo DIGM to form pure-Ni islands; on sanded surfaces, recrystallization produces a high density of grain boundaries that enable extensive DIGM, resulting in several-micrometer-deep interconnected porosity and complete Cr depletion. The central claim is that DIGM is a key mechanism in alloy molten-salt corrosion and that microstructure is a decisive factor in the corrosion response.

Significance. If the mechanistic attribution holds, the work supplies direct comparative evidence that grain-boundary density and DIGM can dominate corrosion morphology over lattice diffusion in molten-salt environments. This would be relevant for surface-preparation protocols and alloy design in chloride-salt systems, and the purely observational, parameter-free character of the study is a methodological strength.

major comments (2)
  1. [Abstract] Abstract: the assertion that the study 'unequivocally establishes DIGM as a key mechanism' and that 'microstructure [is] a decisive contributor' rests on the untested premise that the observed morphological contrast arises solely from recrystallization-induced grain-boundary density. No pre-exposure data are presented on residual stress, surface-oxide thickness/composition, or contamination levels that could independently alter dissolution kinetics.
  2. [Results] Results section (qualitative descriptions of corrosion depths and morphologies): the manuscript reports only qualitative differences in porosity depth and Cr depletion without quantitative diffusion distances, error bars on depletion profiles, or measured grain-boundary densities before versus after exposure. This limits the ability to confirm that DIGM, rather than other sanding-induced effects, accounts for the several-micrometer penetration.
minor comments (1)
  1. [Abstract] The abstract would benefit from a concise statement of the key quantitative observations (e.g., approximate depletion depths or porosity depths) to allow readers to gauge the scale of the DIGM effect.

Simulated Author's Rebuttal

2 responses · 0 unresolved

We thank the referee for their constructive and detailed review of our manuscript. We address each major comment below and describe the revisions we intend to make.

read point-by-point responses

  1. Referee: [Abstract] Abstract: the assertion that the study 'unequivocally establishes DIGM as a key mechanism' and that 'microstructure [is] a decisive contributor' rests on the untested premise that the observed morphological contrast arises solely from recrystallization-induced grain-boundary density. No pre-exposure data are presented on residual stress, surface-oxide thickness/composition, or contamination levels that could independently alter dissolution kinetics.

    Authors: We acknowledge that pre-exposure measurements of residual stress, surface-oxide thickness/composition, and contamination levels were not performed and could in principle influence dissolution kinetics. Our experimental design compares two surface preparations applied to material from the same alloy heat under identical exposure conditions, with the sanding step producing a recrystallized near-surface layer containing a high density of grain boundaries. This contrast allows us to link the enhanced DIGM and porosity to the increased grain-boundary density. We will revise the abstract to replace 'unequivocally establishes' with 'provides strong evidence for' and 'decisive contributor' with 'important contributor,' and we will add a sentence in the discussion section noting the absence of these pre-exposure characterizations as a limitation of the present study. revision: partial

  2. Referee: [Results] Results section (qualitative descriptions of corrosion depths and morphologies): the manuscript reports only qualitative differences in porosity depth and Cr depletion without quantitative diffusion distances, error bars on depletion profiles, or measured grain-boundary densities before versus after exposure. This limits the ability to confirm that DIGM, rather than other sanding-induced effects, accounts for the several-micrometer penetration.

    Authors: The manuscript is observational and focuses on the direct morphological evidence for DIGM (pure-Ni islands above grain boundaries in the electropolished condition and extensive interconnected porosity tied to recrystallized boundaries in the sanded condition). We will add quantitative estimates of grain-boundary density from the provided SEM images and report approximate corrosion depths with reference to multiple fields of view. These additions will help quantify the microstructural difference while preserving the mechanistic emphasis on DIGM. We note that the formation of pure-Ni islands specifically at grain boundaries in the electropolished sample provides direct evidence that DIGM, rather than generic sanding effects, drives the observed sub-surface evolution. revision: yes

Circularity Check

0 steps flagged

No circularity: purely observational comparison without equations or self-referential predictions

full rationale

The paper reports experimental observations of Ni-30Cr alloy corrosion in molten salt under two surface finishes (electropolished vs. sanded), noting layer-by-layer dissolution on electropolished grains versus deep interconnected porosity on sanded surfaces. It attributes the latter to DIGM enabled by recrystallization-induced grain boundaries based on post-exposure microstructure. No equations, fitted parameters, predictions, or derivation chain exist; the central claim rests on direct comparative imaging and interpretation rather than any reduction to inputs by construction or self-citation. This matches the default expectation for non-circular observational work.

Axiom & Free-Parameter Ledger

0 free parameters · 1 axioms · 0 invented entities

The central claim rests on standard materials-science assumptions about grain-boundary diffusion and recrystallization; no free parameters, new entities, or ad-hoc axioms are introduced.

axioms (1)
  • domain assumption Grain boundaries in recrystallized Ni-30Cr act as fast diffusion paths that enable DIGM under the imposed chemical potential gradient from Cr dissolution.
    Invoked to explain why sanded surfaces exhibit deeper attack than electropolished surfaces.

pith-pipeline@v0.9.0 · 5539 in / 1239 out tokens · 34223 ms · 2026-05-10T15:23:27.003056+00:00 · methodology

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Reference graph

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