On the Rheological Memory and Cumulative Damage of Thermoplastic Starch Biodegradable Films Reinforced with Nanoclay

Round 1

Reviewer 1 Report

Comments and Suggestions for Authors

The manuscript examines rheological memory (strain hardening) and cumulative damage of TPS/MMT films using “consecutive vs weekly” cyclic loading and step-stress accelerated life testing modeled with Weibull statistics. I find several substantive issues that must be addressed to support the conclusions; therefore, I recommend Major Revision.

1. Essential experiments should be selectively added to substantiate secondary bond accumulation and junction zone evolution: XRD (d001, intercalation/exfoliation; pre/post-tensile and different hold durations), TEM/SEM or AFM (MMT dispersion/orientation), FTIR/Raman—preferably polarized Raman (hydrogen bonding, TPS–MMT interactions, chain orientation), DMA or time–temperature superposition (E′/E″/tanδ, Tα/Tg, creep/recovery). Add at least two (e.g., XRD + FTIR or TEM + DMA).

2. TPS moisture and RH critically affect strength/fatigue. Specify conditioning/testing T and RH; measure/report moisture content (mean ± SD) and thickness variability; assess moisture/aging changes during weekly intervals. Define whether holds are constant strain or constant load and include representative force–time/strain–time traces to separate relaxation/creep from hardening.

3. The Rheological Memory Index is too narrow. Beyond ultimate strength, report modulus, strain at break, toughness (area under curve), and nonlinear hardening slope (dσ/dε) from full stress–strain curves; quantify Mullins effect/residual strain across cycles. Provide representative curves for “consecutive” vs “weekly” protocols.

4. Benchmarking and application context are limited. Compare (literature-based) to PLA, PBAT, PHA, TPS/PLA, TPS/PBAT for mechanical/fatigue/lifetime; discuss service-relevant stressors (temperature/RH cycling, folding/bending fatigue, puncture, heat-seal zones) and clearly delimit external validity and likely application windows.

5. Add error bars/CI and sample sizes to all plots; detail censoring and failures per step/pattern; perform outlier tests and address Pattern-3 anomalies via replication or justification; consider alternative cumulative damage models (Miner, Basquin/Coffin–Manson, simplified CDM) to demonstrate robustness; provide bootstrap CIs for lifetime parameters.

6. Some minor issues: Justify Weibull over lognormal/loglogistic with physical reasoning (β > 1, increasing hazard, weakest-link); unify stress units to MPa; report MMT surface modification/dispersion stability; justify differing glycerol contents or add controls; correct contradictions on “hold duration vs failure time” and proofread terminology/formatting.

Author Response

Please see the attachment.

Author Response File: Author Response.pdf

Reviewer 2 Report

Comments and Suggestions for Authors

The authors have performed an interesting set of experiments and data analysis in the manuscript titled “On the Rheological Memory and Cumulative Damage of Thermoplastic Starch Biodegradable Films Reinforced with Nano clay”. In the present form the manuscript is poorly written, does not have adequate statistical methods, and lacks severely in terms of presentation of the results. Please find attached my comments.

1. Abstract: rephrase. This is not a lab report and therefore no need to write the aim of the study.
2. Abstract: add data to the abstract, along with P values that indicate the significant differences between samples.
3. Abstract: Most of the abstract is materials and methods and introductions. Please add results and conclusive discussions.
4. Please add line numbers without which it is a wastage of time and resources from the reviewers’ perspective.
5. Introduction: What kind of packaging? food, medical etc. Please be specific. Introduction is super vague. The authors have no idea about the topic related to packaging and waste management and making wild claims and then citing vague sources. Please double check and make sure that you are stating facts, based on research.
6. “Nanomaterials have gained a growing interest” does not have adequate references. It has been studied since long and the idea has been discarded as not being utilizable for packaging. It has no practical applications. Can the authors provide some examples where nanomaterial infused packaging has actually been utilized to make real products?
7. The figures do not have standard deviation bars.
8. Statistical analysis is written in bullet points. Especially the 2.5.2. Do the authors think that this is the correct to present their findings?
9. Statistical analysis lacks the number of replicates used and the method used for detecting significant differences between samples.
10. The axes of figures 1 and 2 are not marked. This is a research manuscript, please make sure that you are doing at least a reasonable effort before submitting. Did the authors even proofread what they wrote?

Author Response

Please see the attachment.

Author Response File: Author Response.pdf

Round 2

Reviewer 2 Report

Comments and Suggestions for Authors

The authors have made the necessary changes. The manuscript has quality has improved.

Author Response

Please see the attachment.

Author Response File: Author Response.pdf