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Multifunctional, Flexible, Electrospun Lignin/PLA Micro/Nanofiber Mats from Softwood Kraft, Hardwood Alcell, and Switchgrass CELF Lignin

This study compares electrospun 1:1 lignin/PLA micro/nanofiber mats from multiple lignin origins and fractions, with water contact angle used as a functional readout for hydrophobicity alongside morphology, thermal, mechanical, and antioxidant measurements.

At-a-Glance Summary

Primary surface measurement reported

Water contact angle of electrospun lignin/PLA fiber mats and a neat PLA control, measured by the sessile drop method under ambient conditions.

Dropometer attribution in the paper

The methods state that water contact angle measurement was carried out using the “Droplet Lab smartphone-based tensiometer (Toronto, ON, Canada)” with the sessile drop method, and the resulting contact angle was calculated using Young–Laplace fitting with automatic Droplet Lab software analysis.

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

The contact-angle data were used to compare hydrophobicity across lignin biomass origins, isolation methods, and fractions within a common 50:50 lignin/PLA electrospinning platform. The authors then interpreted those wettability trends together with hydroxyl-group content, crosslinking behavior, thermal transitions, modulus, and morphology to discuss application-relevant differences among the mats.

Replication / reliability statement

Triplicate measurements were taken within 10 s in three different areas of each sample, and the average contact angle was calculated for each sample.

Paper Details

Title
Multifunctional, Flexible, Electrospun Lignin/PLA Micro/Nanofiber Mats from Softwood Kraft, Hardwood Alcell, and Switchgrass CELF Lignin
Authors
Dorota B. Szlek; Emily L. Fan; Margaret W. Frey
Journal
Fibers
Year
2025
Volume
13
Pages / Article
129
License
CC BY 4.0

Journal context

What it is
Journal-level metrics for the publication venue (not a rating of this specific article).
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Scopus metrics (Elsevier / Scopus rating 2024)

CiteScore 2024

7.4

CiteScore subject ranks (CiteScore 2024)
  • Q1 - Civil and Structural Engineering (66/407)
  • Q1 - Ceramics and Composites (32/130)
  • Q1 - Mechanics of Materials (76/403)
  • Q2 - Biomaterials

Journal Impact Factor (Clarivate JCR)

Journal Impact Factor (JCR 2024)

3.9

5-Year Impact Factor

4.1

JCR category rank

Q2 - Materials Science, Multidisciplinary

What Was Measured

Primary surface / interfacial measurement

The paper reports water contact angle as the surface measurement used to assess hydrophobicity of electrospun 1:1 lignin/PLA mats and a neat PLA control. Average contact-angle values are summarized in Table 3, with representative sessile-drop images shown in Figure 9.

Supporting measurements

The authors also measured suspension conductivity, fiber diameter, fiber morphology by SEM, chemical structure by FTIR, thermal behavior by DSC, mechanical properties by DMA, and antioxidant activity by DPPH reduction/UV-Vis. These measurements were used together with contact angle to interpret how lignin origin, isolation route, and fraction changed fiber performance.

Role of the Dropometer

Water contact angle measurement was carried out under ambient conditions using the Droplet Lab smartphone-based tensiometer and the sessile drop method. A droplet of deionized water was generated on each sample surface using a Hamilton Gastight #1750 syringe fitted with an 18-gauge needle, and the resulting contact angle was calculated using Young–Laplace fitting; the paper also states that Droplet Lab software performed the analysis automatically at the time of measurement collection.

In the study workflow, these Dropometer outputs served as the direct hydrophobicity readout used to compare lignin source, pretreatment method, and fraction within the electrospun 1:1 lignin/PLA system.

Method Snapshot

Method Snapshot Table

Sample Lignin source / fraction Biomass origin / isolation route Dropometer output Instruments Conditions
KL/PLA Kraft lignin as received Softwood / Kraft 131.37 ± 4.56° Droplet Lab smartphone-based tensiometer; Hamilton Gastight #1750 syringe; 18G needle Sessile drop, deionized water, ambient conditions, Young–Laplace fitting, triplicate, 3 areas, within 10 s
AIKL/PLA Acetone-insoluble Kraft lignin Softwood / Kraft fraction 114.47 ± 1.86° Same as above Same as above
ASKL/PLA Acetone-soluble Kraft lignin Softwood / Kraft fraction 126.72 ± 1.14° Same as above Same as above
EIKL/PLA Ethanol-insoluble Kraft lignin Softwood / Kraft fraction 125.66 ± 7.06° Same as above Same as above
ESKL/PLA Ethanol-soluble Kraft lignin Softwood / Kraft fraction 110.62 ± 2.30° Same as above Same as above
ALE40/PLA 40% ethanol-soluble Alcell lignin Hardwood / Alcell organosolv fraction 122.09 ± 6.52° Same as above Same as above
ALE60/PLA 60% ethanol-soluble Alcell lignin Hardwood / Alcell organosolv fraction 138.67 ± 4.37° Same as above Same as above
ALE100/PLA 100% ethanol-soluble Alcell lignin Hardwood / Alcell organosolv fraction 115.76 ± 2.75° Same as above Same as above
ALE100INS/PLA 100% ethanol-insoluble Alcell lignin Hardwood / Alcell organosolv fraction 136.16 ± 5.10° Same as above Same as above
SGL/PLA Switchgrass lignin Switchgrass / CELF 130.26 ± 2.63° Same as above Same as above
PLA Neat PLA control Control 110.75 ± 2.98° Same as above Same as above

Key Findings

Lignin generally increased hydrophobicity

Nearly every lignin/PLA mat showed a higher average water contact angle than neat PLA, which was reported at 110.75 ± 2.98°. The highest tabled values were ALE60/PLA at 138.67 ± 4.37° and ALE100INS/PLA at 136.16 ± 5.10°, with KL/PLA and SGL/PLA also high at 131.37 ± 4.56° and 130.26 ± 2.63°, respectively.

Fraction effects depended on the fractionation route

Within Kraft lignin fractions, ASKL/PLA reached 126.72 ± 1.14° while AIKL/PLA was 114.47 ± 1.86°, and EIKL/PLA reached 125.66 ± 7.06° while ESKL/PLA was 110.62 ± 2.30°. The authors connected these differences to solvent hydrogen-bonding capacity and differences in hydroxyl-group content across the fractions.

Contact-angle trends were interpreted with chemistry and mechanics

The paper reports a moderate inverse correlation between relative total hydroxyl-group content and contact angle (r = −0.43), along with positive relationships between contact angle and higher glass transition temperature (r = 0.45) and Young’s modulus (r = 0.79). In the authors’ interpretation, wettability was therefore tied to OH content, rigidity, and surface roughness of the fiber mats.

Alcell-based mats paired high contact angle with rigidity

ALE60/PLA combined the highest average water contact angle with the highest Young’s modulus and the lowest elongation at break among the mechanically tested mats. The paper also notes that SEM micrographs of Alcell-based fibers showed cracked lignin fiber cores encased in a more flexible PLA skin, reinforcing the distinct structural profile of this group.

Dropometer data fed directly into end-use differentiation

In the conclusions, hydrophobicity was part of the evidence used to distinguish mat families for different applications: SGL/PLA for air filtration, KL/PLA for biomedical and cosmetic-care contexts, and Alcell/PLA for water-filtration and packaging systems. Contact-angle data were one of the functional signals supporting those assignments.

Thresholds / Regimes

The authors explicitly referenced superhydrophobicity as a regime marker at ≥150° when discussing the strongest-performing samples in Section 3.5. In that discussion, ALE60/PLA together with neat KL/PLA and SGL/PLA were identified as the closest systems to this benchmark.
Regime / threshold Value How it was used in the paper Samples linked to the regime in the text Supporting outputs
Superhydrophobicity benchmark ≥150° Used in Section 3.5 to frame the strongest hydrophobic performers as approaching superhydrophobicity ALE60/PLA, KL/PLA, SGL/PLA Table 3; Figure 9

Figures & Visuals

Figure 9 — Representative Dropometer outputs

What it shows

Figure 9 shows example sessile-drop contact-angle images for ESKL/PLA, neat PLA, and ALE60/PLA, giving a visual comparison of lower, baseline, and higher hydrophobic responses within the study.

Figure 6 — Surface morphology context for wettability

What it shows

Figure 6 provides SEM views of selected fiber mats, including ALE60/PLA and SGL/PLA, which the authors discuss alongside rigidity, roughness, and hydrophobic behavior.

Figure 3 — FTIR evidence tied to contact-angle interpretation

What it shows

Figure 3 maps OH-related and monolignol-related FTIR features that the authors later use to interpret differences in thermal behavior and contact angle across the lignin series.

Figure 4 — Crosslinking versus OH-content relationship

What it shows

Figure 4 visualizes the inverse relationship between degree of crosslinking and hydrogen bonding / total OH content, which supports the paper’s chemistry-based reading of wettability trends.

Why It Matters

In this paper, contact angle is one of the functional measurements that separates otherwise similarly processed 1:1 lignin/PLA electrospun mats. Because the electrospinning framework was held constant while lignin source and fraction changed, the Dropometer data gave the authors a direct way to compare how lignin selection shifted surface hydrophobicity across the series.

Those wettability results were then read together with FTIR, DSC, DMA, SEM, conductivity, and antioxidant data to build a fuller property map for the mats. In practical terms, the Dropometer output helped the authors sort which lignin/PLA combinations aligned better with flexible, rigid, barrier-oriented, or multifunctional fiber applications.

Practical Takeaways

Same blend ratio, different wetting outcome

With a fixed 50:50 lignin/PLA formulation and common electrospinning settings, average water contact angle still varied substantially across lignin families and fractions, showing that lignin selection materially changed surface behavior.

Fractionation can tune hydrophobicity

The separation between AIKL/PLA and ASKL/PLA, and between ESKL/PLA and EIKL/PLA, shows that solvent-based fraction choice changed the contact-angle result even within the same Kraft-lignin family.

Alcell fractions delivered the highest tabled contact angles

ALE60/PLA and ALE100INS/PLA provided the top average water contact angles in Table 3, and the paper discusses these materials together with rigidity and barrier-oriented application directions.

Neat KL and SGL already performed strongly

The conclusions emphasize that KL/PLA and SGL/PLA combined strong hydrophobicity with broader functional performance without requiring an extra fractionation step for fiber formation.

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