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Superhydrophobicity mechanism of refoliated quaking aspen leaves after complete defoliation by LDD (gypsy, spongy) moth caterpillars

This paper tracks the wetting behavior of refoliated quaking aspen leaves after complete LDD moth defoliation by measuring water contact angle over time and relating it to leaf surface structure development.

At-a-Glance Summary

Primary surface measurement reported

Water contact angles (WCAs) were measured on the adaxial surface of refoliated quaking aspen leaves during the 2021 refoliation period.

Dropometer attribution in the paper

The Methods attribute WCA measurements to a “contact angle measurement system (Droplet Lab Dropometer).”

How the surface-tension / contact-angle data were used in the study

WCA data were presented as a function of time during the refoliation period and compared against previously reported seasonal wettability datasets to discuss how refoliated leaves develop and maintain non-wettability after budbreak. The WCA results were also discussed alongside SEM observations of evolving microscale papillae and nanoscale epicuticular wax features.

Replication / reliability statement

At least 9 contact angle measurements were conducted per sample, and averages with standard deviations were reported.

Paper Details

Title
Superhydrophobicity mechanism of refoliated quaking aspen leaves after complete defoliation by LDD (gypsy, spongy) moth caterpillars
Authors
Xin Sui; Jason Tam; Harald Keller; Wenyan Liang; Uwe Erb
Journal
Plant Science
Year
2023
Volume
330
Pages / Article
111659
License
© 2023 Elsevier B.V. All rights reserved.

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What Was Measured

Primary surface / interfacial measurement

Water contact angles (WCAs) on the adaxial (upper) leaf surface, measured using deionized water droplets and reported as averages with standard deviations.

Supporting measurements

Leaf size was quantified in two directions (parallel and perpendicular to the midrib) using image-based measurement. Leaf surface morphology development during refoliation was characterized by SEM, including measurements of papillae and epicuticular wax (ECW) feature sizes.

Role of the Dropometer

The “contact angle measurement system (Droplet Lab Dropometer)” was used to measure water contact angles on the adaxial surface of refoliated quaking aspen leaves. Leaves were mounted on 2 × 2 × 0.5 cm plexiglass coupons using double-sided tape, and 10 μL deionized water droplets were dispensed on the leaf surface to obtain WCA values reported as averages with standard deviations. The Methods also note immediate droplet roll-off with slight disturbance during roll-off-angle handling (example: engaging the tilt stage).

In this study, Dropometer-derived WCA data function as the quantitative wetting metric used to track refoliated leaf non-wettability over time and to support comparisons against prior seasonal wettability datasets discussed by the authors.

Method Snapshot

Method Snapshot Table

Sample series (paper context) Leaf collection date(s) Surface measurement output Instruments Conditions (as stated) Notes
Refoliated quaking aspen leaves (2021 refoliation period) July 18, 2021 WCA (average ± standard deviation) contact angle measurement system (Droplet Lab Dropometer) Adaxial leaf surface; leaf mounted on 2 × 2 × 0.5 cm plexiglass coupon with double-sided tape; 10 μL deionized water droplet Optical droplet examples shown in Fig. 2(a)
Refoliated quaking aspen leaves (2021 refoliation period) July 26, 2021 WCA (average ± standard deviation) contact angle measurement system (Droplet Lab Dropometer) Adaxial leaf surface; leaf mounted on 2 × 2 × 0.5 cm plexiglass coupon with double-sided tape; 10 μL deionized water droplet Optical droplet examples shown in Fig. 2(b)
Refoliated quaking aspen leaves (2021 refoliation period) July 31, 2021 WCA (average ± standard deviation) contact angle measurement system (Droplet Lab Dropometer) Adaxial leaf surface; leaf mounted on 2 × 2 × 0.5 cm plexiglass coupon with double-sided tape; 10 μL deionized water droplet Optical droplet examples shown in Fig. 2(c)
Refoliated quaking aspen leaves (2021 refoliation period) August 6, 2021 WCA (average ± standard deviation) contact angle measurement system (Droplet Lab Dropometer) Adaxial leaf surface; leaf mounted on 2 × 2 × 0.5 cm plexiglass coupon with double-sided tape; 10 μL deionized water droplet Optical droplet examples shown in Fig. 2(d)
Refoliated quaking aspen leaves (2021 refoliation period) August 16, 2021 WCA (average ± standard deviation) contact angle measurement system (Droplet Lab Dropometer) Adaxial leaf surface; leaf mounted on 2 × 2 × 0.5 cm plexiglass coupon with double-sided tape; 10 μL deionized water droplet Optical droplet examples shown in Fig. 2(e)
Refoliated quaking aspen leaves (2021 refoliation period) August 26, 2021 WCA (average ± standard deviation) contact angle measurement system (Droplet Lab Dropometer) Adaxial leaf surface; leaf mounted on 2 × 2 × 0.5 cm plexiglass coupon with double-sided tape; 10 μL deionized water droplet Optical droplet examples shown in Fig. 2(f); selected morphology–wetting correlations discussed using Table 1

Key Findings

High-WCA non-wettability during refoliation

During the July 18–August 26, 2021 study period, the paper reports average WCA values ranging from 139.7° ± 3.5° to 150.1° ± 1.9° (summarized in Supplementary Materials S7, Table S2).

Evidence of a superhydrophobic wetting state in mid-to-late July

The Results describe Fig. 2(b–c) as evidence that the leaf surface attained a superhydrophobic wetting state, with a measured WCA > 145°.

Rapid development of high wettability after budbreak in the refoliation case

When comparing refoliated leaves (2021) to an initial growth-stage dataset from 2012, the paper states that leaves collected 2 days after budbreak (July 18, 2021) were already highly hydrophobic, and that the maximum average WCA after 13 days was 150.1° ± 1.9° (Table S2 in Supplementary Materials S7).

Different seasonal trend compared with a normal growth season comparison

In the comparison presented in Fig. 3, the paper reports that refoliated 2021 leaves maintained strong non-wettability until July 31, followed by a slight decrease of WCA in August; this is discussed alongside the seasonal “transition period” described for the 2012 dataset.

WCA discussed alongside multi-scale surface structure development

The paper ties WCA behavior to surface structure development by discussing SEM-observed papillae and epicuticular wax (ECW) morphology through the refoliation period and presenting a correlation table (Table 1) linking micro/nano roughness metrics with wetting properties.

Thresholds / Regimes

The Introduction defines superhydrophobicity using contact-angle and roll-off-angle criteria and frames wettable versus superhydrophobic states using WCA threshold values.

Figures & Visuals

Figure 2 — Representative droplet images across the refoliation period

What it shows

Shows example contact angles of individual water droplets on refoliated leaf surfaces for collection dates spanning July 18 through August 26, 2021.

Figure 3 — Refloiation-period WCA trend compared to a normal-growth season time window

What it shows

Compares average WCAs (with standard deviations) for the 2021 refoliation period against a same-calendar-window dataset from a normal growth season (2012).

Figure 4 — Early growth-stage comparison after budbreak

What it shows

Compares average WCAs (with standard deviations) from the 2021 refoliation period against an initial growth and development phase dataset from 2012.

Why It Matters

In this paper, water contact angle is the primary quantitative metric used to assess non-wettability of refoliated aspen leaves and to track how that wetting behavior evolves across the refoliation period.

By combining Dropometer-based WCA measurements with SEM-based descriptions of papillae and epicuticular wax development, the authors connect wetting behavior to evolving dual-scale surface structure and use comparisons to prior seasonal datasets to frame how refoliation differs from a normal growth season.

Practical Takeaways

Leaf mounting approach for contact-angle testing

The Methods describe mounting leaves on 2 × 2 × 0.5 cm plexiglass coupons using double-sided tape to support WCA measurement on the adaxial surface.

Defined droplet volume and liquid for WCA

The paper reports dispensing 10 μL deionized water droplets for WCA measurements.

Replicate-based reporting of WCA

The paper reports at least 9 contact angle measurements per sample and presents averages with standard deviations.

Time-series wetting characterization during refoliation

WCA measurements were used to track refoliated leaf wetting behavior across multiple collection dates and to support comparisons to previously reported seasonal wettability datasets discussed in the Results.

Low-adhesion handling behavior noted during roll-off-angle attempts

The Methods describe immediate droplet roll-off with slight disturbance during roll-off-angle handling (example: engaging the tilt stage).

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