Thermodynamic stability of twisted domains in AgCrSe$_{2}$ thin films grown on lattice-matched YSZ(111) substrate

Haruto Sato; Jobu Matsuno; Junichi Shiogai; Kazutaka Kudo; Kenshin Inamura; Kota Mihara; Yusuke Tajima

arxiv: 2605.23313 · v1 · pith:5D5HGW2Xnew · submitted 2026-05-22 · ❄️ cond-mat.mtrl-sci · cond-mat.str-el

Thermodynamic stability of twisted domains in AgCrSe₂ thin films grown on lattice-matched YSZ(111) substrate

Haruto Sato , Kota Mihara , Kenshin Inamura , Yusuke Tajima , Kazutaka Kudo , Jobu Matsuno , Junichi Shiogai This is my paper

Pith reviewed 2026-05-25 04:14 UTC · model grok-4.3

classification ❄️ cond-mat.mtrl-sci cond-mat.str-el

keywords AgCrSe2 thin filmstwisted domainsthermodynamic stabilityepitaxial growthpulsed-laser depositiondomain controlpolar orientationsYSZ substrate

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The pith

Critical substrate temperature yields single 60° domain AgCrSe2 thin films on YSZ

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

This paper identifies a critical growth temperature for AgCrSe2 thin films on lattice-matched YSZ(111) that produces only the 60° domain. At temperatures below or above this point, the metastable 0° domain also forms, which the authors attribute to a delicate thermodynamic energy balance. Controlling these domains matters for deploying the material's polar magnetic semiconductor properties in devices without interference from multiple orientations. The work includes surface analysis confirming both +Z and -Z polar directions. The findings suggest similar control is possible for other rhombohedral two-dimensional compounds.

Core claim

Exploring growth temperature and Ag/Cr supply ratio reveals a critical T_sub for single 60° domain in c-axis oriented AgCrSe2 on YSZ(111). Below and above this temperature the 0° domain emerges in addition, indicating the thermodynamic stability balance. Two polar orientations along +Z and -Z are present as shown by time-of-flight low-energy atom scattering spectroscopy.

What carries the argument

Critical substrate temperature T_sub that balances thermodynamic energies to favor single 60° domain over 0° domain.

Load-bearing premise

Observed changes in domain structure with temperature arise from thermodynamic stability of the domains rather than from kinetic limitations or substrate imperfections during deposition.

What would settle it

If the 0° domain fraction stays constant when growth kinetics are slowed by reducing laser repetition rate at non-critical temperatures, the thermodynamic explanation would be supported; variation with rate would point to kinetics instead.

Figures

Figures reproduced from arXiv: 2605.23313 by Haruto Sato, Jobu Matsuno, Junichi Shiogai, Kazutaka Kudo, Kenshin Inamura, Kota Mihara, Yusuke Tajima.

**Figure 3.** Figure 3: FIG. 3 [PITH_FULL_IMAGE:figures/full_fig_p025_3.png] view at source ↗

**Figure 4.** Figure 4: FIG. 4 [PITH_FULL_IMAGE:figures/full_fig_p025_4.png] view at source ↗

**Figure 5.** Figure 5: FIG. 5 [PITH_FULL_IMAGE:figures/full_fig_p025_5.png] view at source ↗

read the original abstract

Control of structural domains in epitaxial thin films of functional materials is a fundamental technique to utilize their intrinsic physical and chemical properties in solid-state devices. In this study, we report on suppression of twisted-domain formation in thin-film growth of polar magnetic semiconductor AgCrSe$_{2}$ using pulsed-laser deposition. In exploring concomitant optimized growth temperature and Ag/Cr composition ratio of supply, we find the critical growth temperature ($T\mathrm{_{sub}}$) for obtaining single 60$^{\circ}$ domain in c-axis oriented AgCrSe$_{2}$ thin film on a lattice-matched (111) plane of the yttria-stabilized zirconia substrate. At temperatures below and above the critical $T\mathrm{_{sub}}$, metastable 0$^{\circ}$ domain in addition to the 60$^{\circ}$ domain emerges, indicating delicate energy balance of thermodynamic stability for obtaining the single-domain structure. Surface structural analysis using time-of-flight low-energy atom scattering spectroscopy reveals the presence of two polar orientations along $+Z$ and $-Z$ directions. These findings provide valuable insights into the thin-film growth mechanisms for a family of two-dimensional compounds with rhombohedral lattices.

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.

Desk Editor's Note private letter to a colleague

The paper reports a specific critical substrate temperature window for single 60° domain AgCrSe2 on YSZ(111) but does not separate thermodynamic stability from kinetic effects in the PLD process.

read the letter

The main thing to know is that the authors found a narrow substrate temperature range, paired with an optimized Ag/Cr ratio, that produces single 60° domain c-axis AgCrSe2 films on lattice-matched YSZ(111). Outside that window, a 0° domain appears alongside it. They also note both +Z and -Z polar orientations via TOF-LEAS. That concrete growth parameter for this material-substrate pair is the new piece; the broader tactic of tuning temperature to suppress twisted domains is already in the literature for other systems. The experimental observation itself looks straightforward and could be useful to groups trying to control domains in similar rhombohedral thin films. The soft spot is the thermodynamic interpretation. The abstract calls the 0° domain metastable and attributes the window to delicate energy balance, yet the data are ex-situ structural checks after growth at different temperatures. PLD kinetics—adatom diffusivity, nucleation barriers, supersaturation—change strongly with temperature, so temperature dependence alone does not isolate thermodynamics from trapping during deposition. No annealing, rate-variation, or in-situ data are referenced that would test whether the 0° orientation can be removed after growth or whether it is simply frozen in. That distinction matters for the central claim. The paper is for experimentalists who grow epitaxial films of 2D polar materials and need practical domain-control recipes. It is not aimed at theorists or at readers seeking broad new mechanisms. I would send it to peer review because the growth result is specific and falsifiable, even if the thermodynamic language needs more support. Reviewers will likely ask for clearer evidence on kinetics versus stability, which is a normal and fixable issue rather than a fatal one.

Referee Report

1 major / 2 minor

Summary. The manuscript reports the growth of c-axis oriented AgCrSe2 thin films on lattice-matched YSZ(111) by pulsed-laser deposition. A critical substrate temperature T_sub is identified at which single 60° domain films are obtained; below and above this temperature a metastable 0° domain appears alongside the 60° domain. The authors attribute the narrow temperature window to a delicate thermodynamic energy balance between the two orientations. Time-of-flight low-energy atom scattering spectroscopy is used to reveal the presence of both +Z and -Z polar surface terminations. The results are presented as providing insights into domain control for rhombohedral 2D compounds.

Significance. If the central claim is substantiated with appropriate controls, the work would demonstrate a practical route to single-domain epitaxial films of a polar magnetic semiconductor and highlight the sensitivity of domain energetics on lattice-matched substrates. Such control is relevant for device applications that rely on the intrinsic polarity and magnetism of AgCrSe2 and related layered materials.

major comments (1)

[Abstract] Abstract: The assertion that the 0° domain is metastable and appears outside the critical T_sub window because of 'delicate energy balance of thermodynamic stability' is not supported by any data that isolate thermodynamics from kinetic effects. No annealing experiments, growth-rate variations, or in-situ monitoring are referenced that would demonstrate the 0° orientation is not simply the result of temperature-dependent adatom mobility or nucleation kinetics during PLD.

minor comments (2)

[Abstract] Abstract: No quantitative metrics (domain population fractions, rocking-curve widths, or error bars) are supplied to support the claim of 'single 60° domain' or the temperature dependence of the 0° domain fraction.
The manuscript would benefit from explicit description of how the 0° and 60° domains were identified and quantified in the structural characterization data.

Simulated Author's Rebuttal

1 responses · 0 unresolved

We thank the referee for the detailed review and constructive criticism. We address the single major comment below.

read point-by-point responses

Referee: [Abstract] Abstract: The assertion that the 0° domain is metastable and appears outside the critical T_sub window because of 'delicate energy balance of thermodynamic stability' is not supported by any data that isolate thermodynamics from kinetic effects. No annealing experiments, growth-rate variations, or in-situ monitoring are referenced that would demonstrate the 0° orientation is not simply the result of temperature-dependent adatom mobility or nucleation kinetics during PLD.

Authors: We agree that the manuscript does not contain direct experiments (annealing, growth-rate series, or in-situ diagnostics) that would rigorously separate thermodynamic stability from kinetic effects during PLD. The claim in the abstract is therefore an interpretation based on the observed non-monotonic temperature dependence: the 0° domain appears on both the low-T and high-T sides of a narrow window for the single 60° domain. Kinetic quantities such as adatom mobility or nucleation rate are expected to vary monotonically with substrate temperature, whereas the existence of a bounded stability window is more naturally explained by a crossing of the free-energy curves of the two orientations. Nevertheless, we accept that this remains an inference rather than a direct demonstration. We will revise the abstract to replace the phrase 'indicating delicate energy balance of thermodynamic stability' with the more cautious wording 'suggesting a narrow temperature window in which the 60° orientation is favored, consistent with a delicate balance between the two domain orientations.' revision: partial

Circularity Check

0 steps flagged

Purely experimental report with no derivations or self-citations

full rationale

The manuscript is an experimental thin-film growth study reporting domain populations observed via ex-situ XRD and TOF-LEAS after PLD at varying T_sub and Ag/Cr ratios. No equations, fitting procedures, ansatzes, or theoretical derivations appear in the text; the central claim is an inference from measured domain fractions rather than a reduction of any quantity to itself by construction. Self-citations are absent from the provided sections, and the interpretation of thermodynamic stability is presented as a qualitative reading of the temperature window, not as a load-bearing mathematical step.

Axiom & Free-Parameter Ledger

0 free parameters · 0 axioms · 0 invented entities

The work is experimental and introduces no free parameters, new axioms, or invented entities. It relies on standard assumptions of epitaxial growth and thermodynamic domain stability.

pith-pipeline@v0.9.0 · 5774 in / 1162 out tokens · 25627 ms · 2026-05-25T04:14:02.407177+00:00 · methodology

discussion (0)

Reference graph

Works this paper leans on

27 extracted references · 27 canonical work pages

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Composition mapping of the surface structure of the sample obtained by high - temperature growth Figure S1 shows scanning electron microscopy (SEM) image and composition mapping obtained by energy dispersive x -ray spectroscopy (EDX) for the film grown at Tsub = 698°C with target Ag/Cr ratio of 6. For the sake of avoiding the effect of substrate, we emplo...

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[1] [1]

Ohkubo, A

I. Ohkubo, A. Ohtomo, T. Ohnishi, Y . Mastumoto, H. Koinuma, M. Kawasaki, In- plane and polar orientations of ZnO thin films grown on atomically flat sapphire , Surf. Sci. 443 L1043 (1999)

work page 1999

[2] [2]

H. W. Jang, D. Ortiz, S. H. Baek, C. M. Folkman, R. R. Das, P. Shafer, Y. Chen, C. T. Nelson, X . Pan, R . Ramesh, C . B. Eom, Domain Engineering for Enhanced Ferroelectric Properties of Epitaxial (001) BiFeO3 Thin Films, Adv. Mater. 21, 817– 823 (2009)

work page 2009

[3] [3]

Bibes, J

M. Bibes, J. E. Villegas, and A. Barthélémy, Ultrathin oxide films and interfaces for electronics and spintronics, Adv. Phys. 60, 5–84 (2011)

work page 2011

[4] [4]

X. Guo, Z. J. Xu, H. C. Liu, B. Zhao, X. Q. Dai, H. T. He, J. N. Wang, H. J. Liu, W. K. Ho, and M. H. Xie, Single domain Bi2Se3 films grown on InP(111)A by molecular- beam epitaxy, Appl. Phys. Lett. 102, 151604 (2013)

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N. V . Tarakina, S. Schreyeck, M. Luysberg, S. Grauer, C. Schumacher, G. Karczewski, K. Brunner, C. Gould, H. Buhmann, R. E. Dunin-Borkowski, and L. W. Molenkamp, Suppressing twin formation in Bi2Se3 thin films, Adv. Mater. Interfaces 1, 1400134 (2014)

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Takahashi, J

K. Takahashi, J. Shiogai, H. Inoue, S. Ito, S. Kimura, S. Awaji, and A. Tsukazaki, 20 Single-domain formation of SrMnBi2 films on polar LaAlO3 substrate, AIP Adv. 10, 105216 (2020)

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Zhang, X

Z. Zhang, X. Yang, K. Liu, and R. Wang, Epitaxy of 2D Materials toward Single Crystals, Adv. Sci. 9, 2105201 (2022)

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Nordlander, M

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work page 2024

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Tajima, J

Y . Tajima, J. Shiogai, M. Ochi, K. Kudo, and J. Matsuno, Engineered substrates for domain control in CrSe thin -film growth: single -domain formation on a lattice - matched YSZ(111) substrate, Jpn. J. Appl. Phys. 64, 065502 (2025)

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Grundmann, T

M. Grundmann, T. Böntgen, and M . Lorenz, Occurrence of rotation domains in heteroepitaxy, Phys. Rev. Lett. 105, 146102 (2010)

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Okada, T

M. Okada, T. Sawazaki, K. Watanabe, T. Taniguchi, H. Hibino, H. Shinohara, and R. Kitaura, Direct Chemical Vapor Deposition Growth of WS 2 Atomic Layers on Hexagonal Boron Nitride, ACS Nano 8, 8273 (2014). 21

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Takahashi, T

H. Takahashi, T. Akiba, A. H. Mayo, K. Akiba, A. Miyake, M. Tokunaga, H. Mori, R. Arita, and S. Ishiwata, Spin -orbit-derived giant magnetoresistance in a layered magnetic semiconductor AgCrSe2, Phys. Rev. Mater. 6, 054602 (2022)

work page 2022

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G. R. Siemann, S. J. Kim, E. A. Morales, P. A. E. Murgatroyd, A. Zivanovic, B. Edwards, I. Markovi ć, F. Mazzola, L. Trzaska, O. J. Clark, C. Bigi, H. Zhang, B. Achinuq, T. Hesjedal, M. D. Watson, T. K. Kim, P. Bencok, G. van der Laan, C. M. Polley, M. Leandersson, H. Fedderwitz, K. Ali, T. Balasubramanian, M. Schmidt, M. Baenitz, H. Rosner, and P. D. C. ...

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Maignan, E

A. Maignan, E. Guilmeau, F. Gascoin, Y. Breard, and V . Hardy, Revisiting some chalcogenides for thermoelectricity, Sci. Technol. Adv. Mater. 13, 053003 (2012)

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D. W. Murphy, H. S. Chen, and B. Tell, Superionic conduction in AgCrS 2 and AgCrSe2, J. Electrochem. Soc. 124, 1268 (1977)

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B. A. Boukamp and G. A. Wiegers, Ionic and electronic processes in AgCrSe2, Solid 22 State Ionics 9-10, 1193 (1983)

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Damay, S

F. Damay, S. Petit, S. Rols, M. Braendlein, R. Daou, E. Elkaïm, F. Fauth, F. Gascoin, C. Martin, and A. Maignan, Localised Ag+ vibrations at the origin of ultralow thermal conductivity in layered thermoelectric AgCrSe2, Sci. Rep. 6, 23415 (2016)

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B. Li, H. Wang, Y . Kawakita, Q. Zhang, M. Feygenson, H. L. Yu, D. Wu, K. Ohara, T. Kikuchi, K. Shibata, T. Yamada, X. K. Ning, Y . Chen, J. Q. He, D. Vaknin, R. Q. Wu, K. Nakajima , and M. G. Kanatzidis , Liquid-like thermal conduction in intercalated layered crystalline solids, Nature Mater. 17, 226 (2018)

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J. Ding, J . L. Niedziela, D . Bansal, J . Wang, X. He, A. F. May, G. Ehlers, D . L. Abernathy, A. Said, A. Alatas, Y. Ren, G. Arya, and O. Delaire, Anharmonic lattice dynamics and superionic transition in AgCrSe 2, Proc. Natl. Acad. Sci. U.S.A. 117, 3930 (2020)

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Tajima, K

Y. Tajima, K. Inamura, S. Masaki, T. Yamazaki, T. Seki, K. Kudo, J. Matsuno, and J. Shiogai, Stoichiometry control and epitaxial growth of AgCrSe2 thin films by pulsed- laser deposition, APL Mater. 13, 061117 (2025)

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Momma and F

K. Momma and F. Izumi, VESTA 3 for three -dimensional visualization of crystal, volumetric and morphology data, J. Appl. Crystallogr. 44, 1272 (2011)

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Z. Sun, Y. Su, A. Zhi, Z. Gao, X. Han, K. Wu, L. Bao, Y. Huang, Y. Shi, X. Bai, P. 23 Cheng, L. Chen, K. Wu, X. Tian, C. Wu, and B. Feng, Evidence for multiferroicity in single-layer CuCrSe2, Nat. Commun. 15, 4252 (2024)

work page 2024

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H. Yu, Z. Yang, L. Du, J. Zhang, J. Shi, W. Chen, P. Chen, M. Liao, J. Zhao, J. Meng, G. Wang, J. Zhu, R. Yang, D. Shi, L. Gu, G. Zhang, Precisely Aligned Monolayer MoS2 Epitaxially Grown on h-BN basal Plane, Small 13, 1603005 (2017). 24 Figure caption FIG. 1. (a)(b) Schematic crystal structures of AgCrSe 2 in (a) low temperature and polar phase in R3m (l...

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For the sake of avoiding the effect of substrate, we employed Al2O3 substrate for composition analysis

Composition mapping of the surface structure of the sample obtained by high - temperature growth Figure S1 shows scanning electron microscopy (SEM) image and composition mapping obtained by energy dispersive x -ray spectroscopy (EDX) for the film grown at Tsub = 698°C with target Ag/Cr ratio of 6. For the sake of avoiding the effect of substrate, we emplo...

work page