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Direct Adhesive Measurements between Wood Biopolyrner Model Surfaces
KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology, Fibre Technology. KTH, School of Chemical Science and Engineering (CHE), Centres, Wallenberg Wood Science Center.
KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology, Polymer Technology.
KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology, Fibre Technology. KTH, School of Chemical Science and Engineering (CHE), Centres, Wallenberg Wood Science Center.ORCID iD: 0000-0001-8622-0386
KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology, Fibre Technology. KTH, School of Chemical Science and Engineering (CHE), Centres, Wallenberg Wood Science Center.ORCID iD: 0000-0002-5444-7276
2012 (English)In: Biomacromolecules, ISSN 1525-7797, E-ISSN 1526-4602, Vol. 13, no 10, 3046-3053 p.Article in journal (Refereed) Published
Abstract [en]

For the first time the dry adhesion was measured for an all-wood biopolymer system using Johnson-Kendall-Roberts (JKR) contact mechanics. The polydimethylsiloxane hemisphere was successfully surface-modified with a Cellulose I model surface using layer-by-layer assembly of nanofibrillated cellulose and polyethyleneimine. Flat surfaces of cellulose were equally prepared on silicon dioxide substrates, and model surfaces of glucomannan and lignin were prepared on silicon dioxide using spin-coating. The measured work of adhesion on loading and the adhesion hysteresis was found to be very similar between cellulose and all three wood polymers, suggesting that the interaction between these biopolymers do not differ greatly. Surface energy calculations from contact angle measurements indicated similar dispersive surface energy components for the model surfaces. The dispersive component was dominating the surface energy for all surfaces. The JKR work of adhesion was lower than that calculated from contact angle measurements, which partially can be ascribed to surface roughness of the model surfaces and overestimation of the surface energies from contact angle determinations.

Place, publisher, year, edition, pages
2012. Vol. 13, no 10, 3046-3053 p.
Keyword [en]
Adhesion, Angle measurement, Biomolecules, Biopolymers, Cellulose, Contact angle, Deformation, Interfacial energy, Loading; Silica, Silicones, Surface roughness
National Category
Chemical Sciences Paper, Pulp and Fiber Technology
Identifiers
URN: urn:nbn:se:kth:diva-104696DOI: 10.1021/bm300762eISI: 000309488600005Scopus ID: 2-s2.0-84867475444OAI: oai:DiVA.org:kth-104696DiVA: diva2:567072
Note

QC 20121112. Updated from Manuscript to Article

Available from: 2012-11-12 Created: 2012-11-09 Last updated: 2017-12-07Bibliographically approved
In thesis
1. Molecular Interactions in Thin Films of Biopolymers, Colloids and Synthetic Polyelectrolytes
Open this publication in new window or tab >>Molecular Interactions in Thin Films of Biopolymers, Colloids and Synthetic Polyelectrolytes
2011 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

The development of the layer-by-layer (LbL) technique has turned out to be an efficient way to physically modify the surface properties of different materials, for example to improve the adhesive interactions between fibers in paper. The main objective of the work described in this thesis was to obtain fundamental data concerning the adhesive properties of wood biopolymers and LbL films, including the mechanical properties of the thin films, in order to shed light on the molecular mechanisms responsible for the adhesion between these materials.

LbLs constructed from poly(allylamine hydrochloride) (PAH)/poly(acrylic acid) (PAA), starch containing LbL films, and LbL films containing nanofibrillated cellulose (NFC) were studied with respect to their adhesive and mechanical properties. The LbL formation was studied using a combination of stagnation point adsorption reflectometry (SPAR) and quartz crystal microbalance with dissipation (QCM-D) and the adhesive properties of the different LbL films were studied in water using atomic force microscopy (AFM) colloidal probe measurements and under ambient conditions using the Johnson-Kendall-Roberts (JKR) approach. Finally the mechanical properties were investigated by mechanical buckling and the recently developed SIEBIMM technique (strain-induced elastic buckling instability for mechanical measurements).

From colloidal probe AFM measurements of the wet adhesive properties of surfaces treated with PAH/PAA it was concluded that the development of strong adhesive joints is very dependent on the mobility of the polyelectrolytes and interdiffusion across the interface between the LbL treated surfaces to allow for polymer entanglements.

Starch is a renewable, cost-efficient biopolymer that is already widely used in papermaking which makes it an interesting candidate for the formation of LbL films in practical systems. It was shown, using SPAR and QCM-D, that LbL films can be successfully constructed from cationic and anionic starches on silicon dioxide and on polydimethylsiloxane (PDMS) substrates. Colloidal probe AFM measurements showed that starch LbL treatment have potential for increasing the adhesive interaction between solid substrates to levels beyond those that can be reached by a single layer of cationic starch. Furthermore, it was shown by SIEBIMM measurements that the elastic properties of starch-containing LbL films can be tailored using different nanoparticles in combination with starch.

LbL films containing cellulose I nanofibrils were constructed using anionic NFC in combination with cationic NFC and poly(ethylene imine) (PEI) respectively. These NFC films were used as cellulose model surfaces and colloidal probe AFM was used to measure the adhesive interactions in water. Furthermore, PDMS caps were successfully coated by LbL films containing NFC which enabled the first known JKR adhesion measurements between cellulose/cellulose, cellulose/lignin and cellulose/glucomannan. The measured adhesion and adhesion hysteresis were similar for all three systems indicating that there are no profound differences in the interaction between different wood biopolymers. Finally, the elastic properties of PEI/NFC LbL films were investigated using SIEBIMM and it was shown that the stiffness of the films was highly dependent on the relative humidity.

Place, publisher, year, edition, pages
Stockholm: KTH Royal Institute of Technology, 2011. ix, 56 p.
Series
TRITA-CHE-Report, ISSN 1654-1081 ; 2011:50
Keyword
Polyelectrolyte multilayers, Layer-by-Layer assembly, Adhesion, Adsorption, Young's modulus, Mechanical buckling, AFM, JKR, SPAR, QCM-D, SIEBIMM, PAH, PAA, Starch, NFC, Nanocellulose
National Category
Materials Chemistry Paper, Pulp and Fiber Technology Nano Technology
Identifiers
urn:nbn:se:kth:diva-41023 (URN)978-91-7501-098-4 (ISBN)
Public defence
2011-10-14, F3, Lindstedtsvägen 26, KTH, Stockholm, 10:00 (English)
Opponent
Supervisors
Note

QC 20110923

Available from: 2011-09-23 Created: 2011-09-23 Last updated: 2014-10-03Bibliographically approved
2. Tailoring adhesion and wetting properties of cellulose fibers and model surfaces
Open this publication in new window or tab >>Tailoring adhesion and wetting properties of cellulose fibers and model surfaces
2012 (English)Licentiate thesis, comprehensive summary (Other academic)
Abstract [en]

The layer-by-layer (LbL) technique was used to modify the surface of cellulose fibers by consecutive adsorption of poly(allylamine hydrochloride) (PAH) and poly(acrylic acid) (PAA) followed by a final adsorbed layer of anionic paraffin wax colloids. Paper hand sheets made from the modified fibers were found to be highly hydrophobic with a contact angle of 150°. In addition to the significantly increased hydrophobicity, the sheets showed improved mechanical properties, such as a higher tensile strength. Heat treatment of the prepared sheets further enhanced both the mechanical properties and the hydrophobicity. These results demonstrate the flexibility and robustness of the LbL technique, which allows us to combine the known adhesive effect of PAH/PAA LbL films with the functionality of wax nanoparticles, creating a stronger and highly hydrophobic paper.

It was further observed that LbL modified sheets without wax also displayed increased hydrophobicity when heat treated. The mechanism was studied through model experiments where LbL films of PAH/PAA were assembled on flat non-porous model cellulose surfaces. Contact angle measurements showed the same trend due to heat treatment of the model films, although, the absolute value of the contact angles were smaller. Analysis using the highly interfacial sensitive vibrational sum frequency spectroscopy technique showed an enrichment of CH3 groups (from the polymer chain ends) at the solid/air interface. These results indicate that during the heat treatment, a reorientation of polymer chains occurs to minimize the surface energy of the LbL film.

In the second part of this work, the adhesive interactions between the main constituents of wood fibers were studied using high-resolution measuring techniques and well-defined model films of cellulose, hemicellulose and lignin. Successful surface modification of polydimethylsiloxane (PDMS) caps, needed in the Johnson-Kendall-Roberts (JKR) measuring methodology, by LbL deposition of nanofibrillated cellulose (NFC) and poly(ethylene imine) (PEI) allowed for the first known all-wood biopolymer JKR measurements of the adhesion between cellulose/cellulose, cellulose/lignin and the cellulose/glucomannan surfaces. The work of adhesion on loading and the adhesion hysteresis were similar for all three systems, suggesting that adhesion between the different wood biopolymers does not differ greatly.

Place, publisher, year, edition, pages
Stockholm: KTH Royal Institute of Technology, 2012. 33 p.
Series
TRITA-CHE-Report, ISSN 1654-1081 ; 2012:8
National Category
Materials Chemistry Paper, Pulp and Fiber Technology Nano Technology
Identifiers
urn:nbn:se:kth:diva-91296 (URN)978-91-7501-268-1 (ISBN)
Presentation
2012-03-19, K1, KTH, Teknikringen 56, Stockholm, 14:00 (English)
Opponent
Supervisors
Note

QC 20120314

Available from: 2012-03-14 Created: 2012-03-12 Last updated: 2014-10-03Bibliographically approved
3. Tailoring Adhesion and Wetting Properties of Cellulose Fibres and Model Surfaces Using Layer-by-Layer Technology
Open this publication in new window or tab >>Tailoring Adhesion and Wetting Properties of Cellulose Fibres and Model Surfaces Using Layer-by-Layer Technology
2014 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

The versatile layer-by-layer (LbL) technique, for consecutive adsorption of polyelectrolytes and charged nanoparticles onto a substrate, was used to modify cellulose fibres and model surfaces for improved mechanical and wetting properties. In addition to being used to modify cellulose substrates, the LbL technique was also used to create cellulose surfaces suitable for high resolution adhesion measurements. LbL assembly of cellulose nanofibrils and polyethylenimine was used to prepare cellulose model surfaces on polydimethylsiloxane hemispheres which allowed for the first known Johnson-Kendall-Roberts (JKR) adhesion measurements between cellulose and smooth, well-defined model surfaces of cellulose, lignin and glucomannan. The work of adhesion on loading and the adhesion hysteresis were comparable for all three systems which suggest that adhesion between wood constituents is similar. The LbL technique was also used to decrease the hydrophilicity of paper, while improving the dry strength, by coating cellulose fibres with a polylallylamine hydrochloride (PAH) and polyacrylic acid (PAA) LbL film, followed by adsorption of anionic wax particles. Paper sheets made from the modified fibres were highly hydrophobic with a contact angle of 150°, while retaining, and in some cases improving, the tensile index of the paper. It was also observed that PAH/PAA modified sheets without the addition of wax became hydrophobic when heat treated. The mechanism behind the increased hydrophobicity was studied by the interface sensitive technique, vibrational sum frequency spectroscopy, which indicated that the increased hydrophobicity is a result of the reorientation of polymer chains to expose more hydrophobic CH2 and CH groups at the polymer-air interface. Paper sheets prepared from LbL-modified bleached softwood fibres using PAH and the biopolymer hyaluronic acid (HA) exhibited a 6.5% strain at break and a tensile index which was increased 3-fold compared to unmodified fibres. The wet adhesive properties of the PAH/HA system were studied by colloidal probe atomic force microscopy and correlated to film growth and viscoelastic behavior. The presence of background salt was a crucial parameter for achieving high adhesion but time in contact and LbL film thickness also strongly affected the adhesion. Finally, the wet adhesive properties of carboxymethylcellulose (CMC), which had been irreversibly adsorbed to regenerated cellulose, and polyvinylamine (PVAm) were evaluated by means of 90° peel tests. Strong wet adhesion was achieved for dried rewetted samples without any obvious chemical crosslinking, which was attributed to interdigitation and complex formation in PVAm-CMC films. This system also gave significant wet adhesion for non-dried systems at water contents around 45%.

Place, publisher, year, edition, pages
Stockholm: KTH Royal Institute of Technology, 2014. vi, 73 p.
Series
TRITA-CHE-Report, ISSN 1654-1081 ; 2014:55
National Category
Polymer Technologies Materials Chemistry Paper, Pulp and Fiber Technology
Research subject
Fibre and Polymer Science
Identifiers
urn:nbn:se:kth:diva-155932 (URN)978-91-7595-347-2 (ISBN)
Public defence
2014-12-04, F3, Lindstedtsvägen 26, KTH, Stockholm, 14:00 (English)
Opponent
Supervisors
Note

QC 20141117

Available from: 2014-11-17 Created: 2014-11-14 Last updated: 2014-11-17Bibliographically approved

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Wågberg, LarsPettersson, Torbjörn

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