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Article
Peer-Review Record

Flux Growth and Characterization of Bulk InVO4 Crystals

Crystals 2023, 13(10), 1439; https://doi.org/10.3390/cryst13101439
by Olesia Voloshyna *, Mikhail V. Gorbunov, Daria Mikhailova, Andrey Maljuk, Silvia Seiro and Bernd Büchner
Reviewer 1:
Reviewer 2: Anonymous
Reviewer 3:
Crystals 2023, 13(10), 1439; https://doi.org/10.3390/cryst13101439
Submission received: 13 September 2023 / Revised: 25 September 2023 / Accepted: 26 September 2023 / Published: 28 September 2023

Round 1

Reviewer 1 Report

Voloshyna et al. reported the flux growth of InVO4 bulk single crystals using copper pyrovanadate as a flux. The obtained InVO4 crystal with a typical size of 0.5*1*7 mm3 has been subjected to a series of characterizations, demonstrating the phase purity, composition, oxidation states, and band gap. Overall, the data are systematic, and the work will contribute to the further study of this material. Therefore, I suggest the publication.

1. The authors performed the cell parameter refinement based on the XRD data of the crushed crystals. However, single-crystal X-ray diffraction measurement is the most powerful technique to determine the crystal structure. Therefore, SCXRD is suggested if the authors want to gain more structural information.

2. The band gap of the InVO4 is determined to be 2.3 eV based on the diffuse reflectance spectrum. The material with such a value of the band gap should appear a yellow color. However, the crystals in this paper look like black, where the band gap should be much less than 2.3 eV. Please explain it.

3. In Figure 5, the authors provide the SEM image of the crystal. Some areas in the crystal are supposed to be the different chemical compositions by EDX. However, no EDX data are presented. Please provide the EDX data.

The writing is concise, but a some sentences are suggested to be further polished.

Author Response

Please, see the attachment

Author Response File: Author Response.pdf

Reviewer 2 Report

Please answer the following question before I considered the manuscript to be published.

a. In the manuscript, you mentioned that the reported eutectic composition of V2O5:InVO4 = 1:1 could not be used as a self-flux. Could you provide more insights into the reasons behind this observation? Did you investigate alternative self-flux compositions or other flux materials? b. The obtained InVO4 crystals were characterized using XRD and X-ray absorption spectroscopy. Could you elaborate on the specific techniques and instruments used for these characterizations? Additionally, did you perform any other structural or morphological analyses on the crystals?

c. The format of the references are not in consistency.

Author Response

Please, see the attachment

Author Response File: Author Response.pdf

Reviewer 3 Report

Flux Growth and Characterization of Bulk InVO4 Crystals

Olesia Voloshyna , Mikhail V. Gorbunov, Daria Mikhailova, Andrey Maljuk, Silvia Seiro, and Bernd Büchner

 Comments of the Referee

The manuscript has been well conceived and can be technically approved. The diagnostical aspects are interesting and can be published in the present form, since they may be very useful for readers. My personal suggestion concerns only the use of a well-known terminology: if I’m not mistaken, it would we worth using the term XRD when working on “single crystals” and XRPD   when “powdered” or “crystal aggregates” are interested in. The Authors know that single crystals are faceted, even if they come from flux growth; on the contrary, one can obtain a perfectly homogeneous crystal phase, like a polycrystalline aggregate, with a well-defined space group.

Very small improvements are needed

Author Response

Please, see the attachment

Author Response File: Author Response.pdf

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