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Cortes Ruiz, M. F., Garemark, J., Ritter, M., Brusentsev, Y., Larsson, P. T., Olsen, P. & Wågberg, L. (2024). Structure-properties relationships of defined CNF single-networks crosslinked by telechelic PEGs. Carbohydrate Polymers, 339, Article ID 122245.
Open this publication in new window or tab >>Structure-properties relationships of defined CNF single-networks crosslinked by telechelic PEGs
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2024 (English)In: Carbohydrate Polymers, ISSN 0144-8617, E-ISSN 1879-1344, Vol. 339, article id 122245Article in journal (Refereed) Published
Abstract [en]

The high structural anisotropy and colloidal stability of cellulose nanofibrils' enable the creation of self-standing fibrillar hydrogel networks at very low solid contents. Adding methacrylate moieties on the surface of TEMPO oxidized CNFs allows the formation of more robust covalently crosslinked networks by free radical polymerization of acrylic monomers, exploiting the mechanical properties of these networks more efficiently. This technique yields strong and elastic networks but with an undefined network structure. In this work, we use acrylate-capped telechelic polymers derived from the step-growth polymerization of PEG diacrylate and dithiothreitol to crosslink methacrylated TEMPO-oxidized cellulose nanofibrils (MATO CNF). This combination resulted in flexible and strong hydrogels, as observed through rheological studies, compression and tensile loading. The structure and mechanical properties of these hydrogel networks were found to depend on the dimensions of the CNFs and polymer crosslinkers. The structure of the networks and the role of individual components were evaluated with SAXS (Small-Angle X-ray Scattering) and photo-rheology. A thorough understanding of hybrid CNF/polymer networks and how to best exploit the capacity of these networks enable further advancement of cellulose-based materials for applications in packaging, soft robotics, and biomedical engineering.

Place, publisher, year, edition, pages
Elsevier BV, 2024
Keywords
Cellulose nanofibrils, Hydrogel, Nanostructure, Network, Polymerization
National Category
Polymer Chemistry
Identifiers
urn:nbn:se:kth:diva-347042 (URN)10.1016/j.carbpol.2024.122245 (DOI)001241667800001 ()38823913 (PubMedID)2-s2.0-85193906068 (Scopus ID)
Note

QC 20240626

Available from: 2024-05-30 Created: 2024-05-30 Last updated: 2024-06-26Bibliographically approved
Garemark, J., Ram, F., Liu, L., Sapouna, I., Cortes Ruiz, M. F., Larsson, P. T. & Li, Y. (2023). Advancing Hydrovoltaic Energy Harvesting from Wood through Cell Wall Nanoengineering. Advanced Functional Materials, 33, 2208933
Open this publication in new window or tab >>Advancing Hydrovoltaic Energy Harvesting from Wood through Cell Wall Nanoengineering
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2023 (English)In: Advanced Functional Materials, ISSN 1616-301X, E-ISSN 1616-3028, Vol. 33, p. 2208933-Article in journal (Refereed) Published
Abstract [en]

Converting omnipresent environmental energy through the assistance of spontaneous water evaporation is an emerging technology for sustainable energy systems. Developing bio-based hydrovoltaic materials further pushes the sustainability, where wood is a prospect due to its native hydrophilic and anisotropic structure. However, current wood-based water evaporation-assisted power generators are facing the challenge of low power density. Here, an efficient hydrovoltaic wood power generator is reported based on wood cell wall nanoengineering. A highly porous wood with cellulosic network filling the lumen is fabricated through a green, one-step treatment using sodium hydroxide to maximize the wood surface area, introduce chemical functionality, and enhance the cell wall permeability of water. An open-circuit potential of ≈140 mV in deionized water is realized, over ten times higher than native wood. Further tuning the pH difference between wood and water, due to an ion concentration gradient, a potential up to 1 V and a remarkable power output of 1.35 µW cm−2 is achieved. The findings in this study provide a new strategy for efficient wood power generators.

Keywords
cell wall nanoengineering, green chemistry, water evaporation, wood power generators
National Category
Materials Chemistry
Identifiers
urn:nbn:se:kth:diva-319626 (URN)10.1002/adfm.202208933 (DOI)000889903100001 ()2-s2.0-85142365851 (Scopus ID)
Funder
Knut and Alice Wallenberg Foundation, 742733Swedish Research Council, 2017‐05349
Note

QC 20230512

Available from: 2022-10-04 Created: 2022-10-04 Last updated: 2023-05-12Bibliographically approved
Sellman, F. A., Benselfelt, T., Larsson, P. T. & Wågberg, L. (2023). Hornification of cellulose-rich materials: A kinetically trapped state. Carbohydrate Polymers, 318, Article ID 121132.
Open this publication in new window or tab >>Hornification of cellulose-rich materials: A kinetically trapped state
2023 (English)In: Carbohydrate Polymers, ISSN 0144-8617, E-ISSN 1879-1344, Vol. 318, article id 121132Article in journal (Refereed) Published
Abstract [en]

The fundamental understanding concerning cellulose-cellulose interactions under wet and dry conditions remains unclear. This is especially true regarding the drying-induced association of cellulose, commonly described as an irreversible phenomenon called hornification. A fundamental understanding of the mechanisms behind hornification would contribute to new drying techniques for cellulose-based materials in the pulp and paper industry while at the same time enhancing material properties and facilitating the recyclability of cellulose-rich materials. In the present work, the irreversible joining of cellulose-rich surfaces has been studied by subjecting cellulose nanofibril (CNF) films to different heat treatments to establish a link between reswelling properties, structural characteristics as well as chemical and mechanical analyses. A heating time/temperature dependence was observed for the reswelling of the CNF films, which is related to the extent of hornification and is different for different chemical compositions of the fibrils. Further, the results indicate that hornification is related to a diffusion process and that the reswellability increases very slowly over long time, indicating that equilibrium is not reached. Hence, hornification is suggested to be a kinetically limited phenomenon governed by non-covalent reversible interactions and a time/temperature dependence on their forming and breaking.

Place, publisher, year, edition, pages
Elsevier BV, 2023
Keywords
Aggregation, Cellulose nanofibril, Hornification, Kinetics, Swelling
National Category
Materials Chemistry Paper, Pulp and Fiber Technology
Identifiers
urn:nbn:se:kth:diva-334855 (URN)10.1016/j.carbpol.2023.121132 (DOI)001056626000001 ()37479442 (PubMedID)2-s2.0-85163374088 (Scopus ID)
Note

QC 20230829

Available from: 2023-08-28 Created: 2023-08-28 Last updated: 2024-05-07Bibliographically approved
Esteves, C., Brännvall, E., Stevanic, J. S. & Larsson, P. T. (2023). Pulp delignification and refining: impact on the supramolecular structure of softwood fibers. Cellulose, 30(16), 10453-10468
Open this publication in new window or tab >>Pulp delignification and refining: impact on the supramolecular structure of softwood fibers
2023 (English)In: Cellulose, ISSN 0969-0239, E-ISSN 1572-882X, Vol. 30, no 16, p. 10453-10468Article in journal (Refereed) Published
Abstract [en]

The effect on softwood fiber wall nanostructure of kraft cooking, oxygen delignification and refining was evaluated by X-ray scattering. A recently developed simulation method for modelling small angle X-ray scattering (SAXS) data was used to estimate the apparent average sizes of solids (AAPS) and interstitial spaces in the fiber wall (AACS). Fiber saturation point and wide angle X-ray scattering were also used to calculate the pore volume in the fiber wall and the crystallite size of the fibril, respectively. The experimental modelled SAXS data was able to give consistent values for each kraft-cooked and oxygen-delignified pulp. Kraft delignification seems to have the major influence on the fiber nanostructure modification, while oxygen delignification has little or no significant impact even for different kappa numbers. The particle sizes values were more stable than the cavities sizes and no significant differences were seen between different delignification processes, refining or delignification degree. Pulps evaluated after PFI-refining, showed an increase in the fiber wall porosity evaluated by FSP and an increase in the interstitial spaces in the fiber wall, while the crystallite size and the particle sizes were very little or not affected at all.

Place, publisher, year, edition, pages
Springer Nature, 2023
Keywords
FSP, Kraft cooking, Oxygen delignification, Refining, SAXS, WAXS
National Category
Paper, Pulp and Fiber Technology
Identifiers
urn:nbn:se:kth:diva-349829 (URN)10.1007/s10570-023-05490-4 (DOI)001065952300001 ()2-s2.0-85171308873 (Scopus ID)
Note

QC 20240703

Available from: 2024-07-03 Created: 2024-07-03 Last updated: 2024-07-03Bibliographically approved
Larsson, P. T., Stevanic-Srndovic, J., Roth, S. V. & Söderberg, D. (2022). Interpreting SAXS data recorded on cellulose rich pulps. Cellulose, 29(1), 117-131
Open this publication in new window or tab >>Interpreting SAXS data recorded on cellulose rich pulps
2022 (English)In: Cellulose, ISSN 0969-0239, E-ISSN 1572-882X, Vol. 29, no 1, p. 117-131Article in journal (Refereed) Published
Abstract [en]

A simulation method was developed for modelling SAXS data recorded on cellulose rich pulps. The modelling method is independent of the establishment of separate form factors and structure factors and was used to model SAXS data recorded on dense samples. An advantage of the modelling method is that it made it possible to connect experimental SAXS data to apparent average sizes of particles and cavities at different sample solid contents. Experimental SAXS data could be modelled as a superposition of a limited number of simulated intensity components and gave results in qualitative agreement with CP/MAS 13C-NMR data recorded on the same samples. For the water swollen samples, results obtained by the SAXS modelling method and results obtained from CP/MAS 13C-NMR measurements, agreed on the ranking of particle sizes in the different samples. The SAXS modelling method is dependent on simulations of autocorrelation functions and the time needed for simulations could be reduced by rescaling of simulated correlation functions due to their independence of the choice of step size in real space. In this way an autocorrelation function simulated for a specific sample could be used to generate SAXS intensity profiles corresponding to all length scales for that sample and used for efficient modelling of the experimental data recorded on that sample. Graphical abstract: [Figure not available: see fulltext.]

Place, publisher, year, edition, pages
Springer Nature, 2022
Keywords
Cellulose, CP/MAS 13C-NMR, FSP; Pulp, Modelling, SAXS, Autocorrelation, 13C NMR, Autocorrelation functions, Form factors, FSP;, Model method, Modeling, SAXS modeling, Structure factors, Data, Intensity, Nuclear Magnetic Resonance, Particles, Pulps, Samples, Shape
National Category
Other Chemistry Topics Other Chemical Engineering
Identifiers
urn:nbn:se:kth:diva-313171 (URN)10.1007/s10570-021-04291-x (DOI)000716892300001 ()2-s2.0-85118838145 (Scopus ID)
Note

QC 20220602

Available from: 2022-06-02 Created: 2022-06-02 Last updated: 2022-09-23Bibliographically approved
Görür, Y. C., Reid, M. S., Montanari, C., Larsson, P. T., Larsson, P. A. & Wågberg, L. (2021). Advanced Characterization of Self-Fibrillating Cellulose Fibers and Their Use in Tunable Filters. ACS Applied Materials and Interfaces, 13(27), 32467-32478
Open this publication in new window or tab >>Advanced Characterization of Self-Fibrillating Cellulose Fibers and Their Use in Tunable Filters
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2021 (English)In: ACS Applied Materials and Interfaces, ISSN 1944-8244, E-ISSN 1944-8252, Vol. 13, no 27, p. 32467-32478Article in journal (Refereed) Published
Abstract [en]

Thorough characterization and fundamental understanding of cellulose fibers can help us develop new, sustainable material streams and advanced functional materials. As an emerging nanomaterial, cellulose nanofibrils (CNFs) have high specific surface area and good mechanical properties; however, handling and processing challenges have limited their widespread use. This work reports an in-depth characterization of self-fibrillating cellulose fibers (SFFs) and their use in smart, responsive filters capable of regulating flow and retaining nanoscale particles. By combining direct and indirect characterization methods with polyelectrolyte swelling theories, it was shown that introduction of charges and decreased supramolecular order in the fiber wall were responsible for the exceptional swelling and nanofibrillation of SFFs. Different microscopy techniques were used to visualize the swelling of SFFs before, during, and after nanofibrillation. Through filtration and pH adjustment, smart filters prepared via in situ nanofibrillation showed an ability to regulate the flow rate through the filter and a capacity of retaining 95% of 300 nm (diameter) silica nanoparticles. This exceptionally rapid and efficient approach for making smart filters directly addresses the challenges associated with dewatering of CNFs and bridges the gap between science and technology, making the widespread use of CNFs in high-performance materials a not-so-distant reality.

Place, publisher, year, edition, pages
American Chemical Society (ACS), 2021
National Category
Paper, Pulp and Fiber Technology
Identifiers
urn:nbn:se:kth:diva-310565 (URN)10.1021/acsami.1c06452 (DOI)000674333400112 ()34106700 (PubMedID)2-s2.0-85108603778 (Scopus ID)
Note

QC 20220406

Available from: 2022-04-04 Created: 2022-04-04 Last updated: 2024-03-15Bibliographically approved
Jawerth, M., Brett, C., Terrier, C., Larsson, P. T., Lawoko, M., Roth, S. V., . . . Johansson, M. (2020). Mechanical and Morphological Properties of Lignin-Based Thermosets. ACS APPLIED POLYMER MATERIALS, 2(2), 668-676
Open this publication in new window or tab >>Mechanical and Morphological Properties of Lignin-Based Thermosets
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2020 (English)In: ACS APPLIED POLYMER MATERIALS, ISSN 2637-6105, Vol. 2, no 2, p. 668-676Article in journal (Refereed) Published
Abstract [en]

The need for renewable alternatives for fossil-based aromatic material constituents is evident for a more sustainable society. Lignin is the largest source of naturally occurring aromatic compounds but has mainly been considered as waste material or energy source in the pulp and paper industry. Developments in extracting lignin from these processes provide a large source for renewable aromatic structures to be used in various applications. Producing thermosets out of lignin is a very promising route to utilize this raw material toward, for example, composite application. The buildup of the molecular network based on oligomeric lignin segments will be different from traditional thermoset analogues, where the constituents often are smaller molecules, and will have an effect on the material properties. In this work LignoBoost Kraft lignin is refined, chemically modified, and used to produce freestanding thermosets with different architectures and properties. These different thermosets are evaluated, and the possibilities to tailor the material properties through work-up and modification are demonstrated. Morphological studies on the formed thermosets using X-ray scattering show systematic differences in molecular stacking and aggregate sizes.

Place, publisher, year, edition, pages
AMER CHEMICAL SOC, 2020
Keywords
lignin fractions, aryl allyl ethers, thiol-ene thermoset, mechanical properties, small- and wide-angle X-ray scattering
National Category
Paper, Pulp and Fiber Technology
Identifiers
urn:nbn:se:kth:diva-271305 (URN)10.1021/acsapm.9b01007 (DOI)000514258700059 ()2-s2.0-85085968247 (Scopus ID)
Note

QC 20200331

Available from: 2020-03-31 Created: 2020-03-31 Last updated: 2022-09-13Bibliographically approved
Mianehrow, H., Lo Re, G., Carosio, F., Fina, A., Larsson, P. T., Chen, P. & Berglund, L. (2020). Strong reinforcement effects in 2D cellulose nanofibril-graphene oxide (CNF-GO) nanocomposites due to GO-induced CNF ordering. Journal of Materials Chemistry A, 8(34), 17608-17620
Open this publication in new window or tab >>Strong reinforcement effects in 2D cellulose nanofibril-graphene oxide (CNF-GO) nanocomposites due to GO-induced CNF ordering
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2020 (English)In: Journal of Materials Chemistry A, ISSN 2050-7488, E-ISSN 2050-7496, Vol. 8, no 34, p. 17608-17620Article in journal (Refereed) Published
Abstract [en]

Nanocomposites from native cellulose with low 2D nanoplatelet content are of interest as sustainable materials combining functional and structural performance. Cellulose nanofibril-graphene oxide (CNF-GO) nanocomposite films are prepared by a physical mixing-drying method, with a focus on low GO content, the use of very large GO platelets (2-45 mu m) and nanostructural characterization using synchrotron X-ray source for WAXS and SAXS. These nanocomposites can be used as transparent coatings, strong films or membranes, as gas barriers or in laminated form. CNF nanofibrils with random in-plane orientation, form a continuous non-porous matrix with GO platelets oriented in-plane. GO reinforcement mechanisms in CNF are investigated, and relationships between nanostructure and suspension rheology, mechanical properties, optical transmittance and oxygen barrier properties are investigated as a function of GO content. A much higher modulus reinforcement efficiency is observed than in previous polymer-GO studies. The absolute values for modulus and ultimate strength are as high as 17 GPa and 250 MPa at a GO content as small as 0.07 vol%. The remarkable reinforcement efficiency is due to improved organization of the CNF matrix; and this GO-induced mechanism is of general interest for nanostructural tailoring of CNF-2D nanoplatelet composites.

Place, publisher, year, edition, pages
Royal Society of Chemistry (RSC), 2020
National Category
Biomaterials Science
Identifiers
urn:nbn:se:kth:diva-282261 (URN)10.1039/d0ta04406g (DOI)000566092600024 ()33796318 (PubMedID)2-s2.0-85090791547 (Scopus ID)
Note

QC 20201030

Available from: 2020-10-30 Created: 2020-10-30 Last updated: 2022-08-31Bibliographically approved
Karlsson, P.-M. R., Larsson, P. T., Pettersson, T. & Wågberg, L. (2020). Swelling of Cellulose-Based Fibrillar and Polymeric Networks Driven by Ion-Induced Osmotic Pressure. Langmuir, 36(41), 12261-12271
Open this publication in new window or tab >>Swelling of Cellulose-Based Fibrillar and Polymeric Networks Driven by Ion-Induced Osmotic Pressure
2020 (English)In: Langmuir, ISSN 0743-7463, E-ISSN 1520-5827, Vol. 36, no 41, p. 12261-12271Article in journal (Refereed) Published
Abstract [en]

Cellulose-based model materials in the form of fibrillar networks and macromolecular hydrogels were used to investigate the ion-induced swelling in relation to the elasticity and structure of the network. Both networks were charged by the introduction of carboxyl groups onto the cellulose surface, and the dimensions of the networks in aqueous solution were measured as a function of pH. The use of cellulose-model materials that contained either noncrystalline cellulose or cellulose I fibrils made it possible to model the effect of the ion-induced osmotic pressure of a delignified wood fiber wall. The noncrystalline hydrogels represented the noncrystalline domains of the fiber wall and the fibrillar network represented the supramolecular network of cellulose I fibrils of the fiber wall. The experimental results were compared to swelling potentials computed using the Donnan theory, and it was found that the ion-induced water uptake within the cellulose networks followed the theoretical predictions to a large extent. However, fibrillar networks were found to plastically deform upon swelling and deviated from the ideal Donnan theory for polyelectrolyte gel networks. Upon addition of salt to the aqueous phase surrounding the cellulose materials, both hydrogels and fibrillar networks deviated from the Donnan theory predictions, suggesting that structural differences between the networks impact their swelling.

Place, publisher, year, edition, pages
American Chemical Society (ACS), 2020
National Category
Chemical Sciences
Identifiers
urn:nbn:se:kth:diva-287393 (URN)10.1021/acs.langmuir.0c02051 (DOI)000584421100018 ()32986431 (PubMedID)2-s2.0-85093876393 (Scopus ID)
Note

QC 20201215

Available from: 2020-12-15 Created: 2020-12-15 Last updated: 2022-11-30Bibliographically approved
Ottesen, V., Larsson, P. T., Chinga-Carrasco, G., Syverud, K. & Gregersen, O. W. (2019). Mechanical properties of cellulose nanofibril films: effects of crystallinity and its modification by treatment with liquid anhydrous ammonia. Cellulose, 26(11), 6615-6627
Open this publication in new window or tab >>Mechanical properties of cellulose nanofibril films: effects of crystallinity and its modification by treatment with liquid anhydrous ammonia
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2019 (English)In: Cellulose, ISSN 0969-0239, E-ISSN 1572-882X, Vol. 26, no 11, p. 6615-6627Article in journal (Refereed) Published
Abstract [en]

The influence of cellulose crystallinity on mechanical properties of cellulose nano-fibrils (CNF) was investigated. Degree of crystallinity (DoC) was modified using liquid anhydrous ammonia. Such treatment changes crystal allomorph from cellulose I to cellulose III, a change which was reversed by subsequent boiling in water. DoC was measured using solid state nuclear magnetic resonance (NMR). Crystalline index (CI) was also measured using wide angle X-ray scattering (WAXS). Cotton linters were used as the raw material. The cotton linter was ammonia treated prior to fibrillation. Reduced DoC is seen to associate with an increased yield point and decreased Young modulus. Young modulus is here defined as the maximal slope of the stress-strain curves. The association between DoC and Young modulus or DoC and yield point are both statistically significant. We cannot conclude there has been an effect on strainability. While mechanical properties were affected, we found no indication that ammonia treatment affected degree of fibrillation. CNF was also studied in air and liquid using atomic force microscopy (AFM). Swelling of the nanofibers was observed, with a mean diameter increase of 48.9%.

Place, publisher, year, edition, pages
SPRINGER, 2019
Keywords
Degree of crystallinity, Mechanical properties, Swelling, Cellulose nanofibrils
National Category
Polymer Technologies
Identifiers
urn:nbn:se:kth:diva-255426 (URN)10.1007/s10570-019-02546-2 (DOI)000473598400013 ()2-s2.0-85067190175 (Scopus ID)
Note

QC 20190815

Available from: 2019-08-15 Created: 2019-08-15 Last updated: 2022-06-26Bibliographically approved
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ORCID iD: ORCID iD iconorcid.org/0000-0001-9176-7116

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