Ion‐Mediated Gelation of Thermo‐Responsive Cellulose Nanofibril/Poly(N‐isopropylacrylamide) Hybrid Hydrogels with Tunable De‐Swelling Kinetics
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Abstract The tunability of the lower critical solution temperature (LCST) of poly(N‐isopropylacrylamide) (PNIPAM) to lower or higher temperatures, as well as the ease of modulation of the LCST phase transition kinetics broadens the scope of application of PNIPAM‐based materials in biomedical fields. This work reports a facile approach to formulate a smart, injectable cellulose nanofibril (CNF)/PNIPAM hybrid gel. Hofmeister salts are used to induce ion‐mediated gelation of the nanofibrils and PNIPAM chains, resulting in an interpenetrating network (IPN) structure. From rheological measurements, the hybrid material displays excellent structural integrity at room temperature and tunable thermo‐stiffening around body temperature. De‐swelling kinetics can be modulated by varying the nature and concentration of the Hofmeister ion used. The successful realization of the IPN hybrid gel structure is dependent on the molecular weight of PNIPAM used. Moreover, the hybrid gels show good thermo‐reversibility during thermal cycling, as well as excellent injectability and remarkable self‐healing post‐injection, owing to shear‐thinning and thixotropic characters. Since rheology is a crucial technique in the analysis of soft matter and flow behavior is fundamental for the design and synthesis of application‐specific viscoelastic materials, the work reported herein provides a rheological basis for careful design and synthesis of smart gels.
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CNFs are extracted through mechanical fibrillation methods including high-pressure homogenization and grinding, often aided by chemical or enzymatic pre-treatments such as TEMPO-mediated oxidation to enhance fibrillation efficiency and reduce energy demand.
“CNFs (Figure 3b), on the other hand, are extracted through mechanical fibrillation methods including high-pressure homogenization and grinding, often aided by chemical or enzymatic pre-treatments such as 2,2,6,6-tetramethylpiperidine-1-oxyl (TEMPO)-mediated oxidation to enhance fibrillation efficiency and reduce energy demand [58,59,60]”
From Nanocellulose-Reinforced Poly(Lactic Acid) and Poly(ε-caprolactone) Bio-Nanocomposites: A Review and Future Outlook for Poly(Lactic Acid)/Poly(ε-caprolactone) Blend Systems (2025) · cites this paper as [60]
The Results and Discussion and Experimental Section (pages not provided) describe TEMPO oxidation followed by low-energy sonication to isolate CNFs. They do not describe high-pressure homogenization, grinding, or enzymatic pretreatment, or establish that the pretreatment improves fibrillation efficiency or reduces energy demand relative to other methods. (LLM, conf=0.88)
Experimental — accuracy not yet measuredFTIR shows characteristic cellulose bands at ~3340 cm−1 (O-H stretching), ~2900 cm−1 (C-H stretching), and ~1050 cm−1 (C-O-C stretching), with additional peaks in modified NC indicating successful surface functionalization.
“The literature reports characteristic cellulose bands at ~3340 cm−1 (O–H stretching), ~2900 cm−1 (C–H stretching), and ~1050 cm−1 (C–O–C stretching), with additional peaks in modified NC, indicating successful surface functionalization [23,60]”
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Cited by
Sorted by citations
Ngwenya, M., Gumede, T. P., Pérez Camargo, R. A., & Motloung, B. (2025) · Materials · doi:10.3390/ma18225172 · Cited by 9 · see citing works
“…are extracted through mechanical fibrillation methods including high-pressure homogenization and grinding, often aided by chemical or enzymatic pre-treatments such as 2,2,6,6-tetramethylpiperidine-1-oxyl (TEMPO)-mediated oxidation to enhance fibrillation efficiency and reduce energy demand [58–60].”
Self-citation
- Authors
- Motloung, B., Pfukwa, R., & Klumperman, B.
- Affiliations
- Stellenbosch University (ZA)
- Corresponding author
- Pfukwa, Rueben
- Klumperman, Bert
- Venue
- Macromolecular Materials and Engineering
- Publisher
- Wiley
- Published
- 2024-05-16
- Volume
- 309
- Issue
- 8
- ISSN
- 1438-7492 (ISSN-L)
- 1439-2054
- OpenAlex
- W4396954843
- Cited by
- 19
- References
- 73
- Citations by year
- 2026: 10 · 2025: 8 · 2024: 1
- FWCI
- 2.37
- Type
- journal article
- Language
- en
- Open access
- gold
- doi.org
- Licence
- Locations
- Macromolecular Materials and Engineering (publishedVersion, cc-by)
- DOAJ (DOAJ: Directory of Open Access Journals) (submittedVersion)
- Funders
- National Research Foundation (102586)
- Topics
- Life Sciences › Biochemistry, Genetics and Molecular Biology › Molecular Medicine › Hydrogels: synthesis, properties, applications
- Physical Sciences › Materials Science › Biomaterials › Advanced Cellulose Research Studies
- Physical Sciences › Materials Science › Biomaterials › Supramolecular Self-Assembly in Materials
- Keywords
- cellulose nanofibers, poly(N-isopropylacrylamide), hybrid hydrogels, lower critical solution temperature, thermosensitive hydrogel, interpenetrating polymer networks, injectable hydrogel, self-healing, shear thinning, thixotropy, molecular weight effects
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