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Friction and forces between cellulose model surfaces: A comparison
KTH, School of Chemical Science and Engineering (CHE), Chemistry, Surface Chemistry.
KTH, School of Chemical Science and Engineering (CHE), Chemistry, Surface Chemistry.
KTH, School of Chemical Science and Engineering (CHE), Fibre and Polymer Technology.ORCID iD: 0000-0001-8622-0386
KTH, School of Biotechnology (BIO), Centres, Albanova VinnExcellence Center for Protein Technology, ProNova.
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2006 (English)In: Journal of Colloid and Interface Science, ISSN 0021-9797, E-ISSN 1095-7103, Vol. 303, no 1, 117-123 p.Article in journal (Refereed) Published
Abstract [en]

Four different cellulose model surfaces, and one silica surface, have been studied by means of atomic force microscopy (AFM). The normal interactions have been found to consist of a longer range double layer force with a short range steric interaction, the nature of which is extensively discussed. Both the surface charge and range of the steric force depend on the type of cellulose substrate used, as does the magnitude of the adhesion. Studies of friction reveal that surface roughness is the determining factor for the friction coefficient, with which it increases monotonically. The absolute value, however, is determined by the surface chemistry. All studied cellulose surfaces show similar behavior in response to xyloglucan addition.

Place, publisher, year, edition, pages
2006. Vol. 303, no 1, 117-123 p.
Keyword [en]
AFM; cellulose; surface forces; colloid probe; xyloglucan; nanotrilology; friction
National Category
Physical Chemistry
Identifiers
URN: urn:nbn:se:kth:diva-7721DOI: 10.1016/j.jcis.2006.06.070ISI: 000241079500015Scopus ID: 2-s2.0-33748919455OAI: oai:DiVA.org:kth-7721DiVA: diva2:12831
Note
QC 20100804Available from: 2007-11-25 Created: 2007-11-25 Last updated: 2017-12-14Bibliographically approved
In thesis
1. Probing Interactions between Bio-Fibre Components
Open this publication in new window or tab >>Probing Interactions between Bio-Fibre Components
2007 (English)Licentiate thesis, comprehensive summary (Other scientific)
Abstract [sv]

I den här avhandlingen har atomkrafts mikroskopi (AFM) och kvartskristall mikrovåg med dissipation (QCM-D) används för att undersöka interaktioner i bio-fiber modell system av cellulosa och xyloglukan (XG); en naturligt förekommande polysackarid viktig för tillväxt av träd och andra växter. Dessutom har det avgörande momentet av friktionskrafts-kalibrering studerats för att erhålla noggranna och kvantitativa resultat med kolloidal prob AFM.

Fyra olika cellulosa modell ytor med varierande morfologi har utvärderats med kolloidal prob AFM. De normala ytkrafterna för alla undersökta substrat var kvalitativt likadana. Däremot, för en given ytråhet leder adsorption av XG till en konsekvent reduktion av friktions-koefficienterna för alla ytor, vilket antyder att effekten på friktion av antingen ytråhet eller kemi kan separeras. För att kunna undersöka interaktionen mellan enbart cellulosa och xyloglukan ändmodifierades först XG enzymatiskt med en tiol grupp. Dessa makromolekyler ympades sedan till guld, där de bildade ett tiol-bundet borst-liknande lager. QCM-D experiment bekräftade att det ympade lagret var biologiskt tillgängligt för enzymatisk nedbrytning genom användning av växtenzymet endo-xyloglukanas TmNXG1. Friktions-koefficienterna för den orörda ympningen och den enzymexponerade visade samma trend med ytråheten som i fallet med cellulosaytorna. Adhesions mätningar på denna modellyta visade att den ursprungliga specificiteten mellan xyloglukan och cellulosa bevarades.

Ett antal AFM kantilevrar har kalibrerats med olika tekniker för att erhålla både normal- och friktionsfjäder-konstanter med mål att utvärdera den relativa noggrannheten mellan de olika metoderna. Överensstämmelsen var god mellan teknikerna för att bestämma fjäder konstanterna i normalled. Något högre avvikelse mellan teknikerna för att bestämma torsions fjäder konstanterna förekom. Men denna avvikelse leder inte till kvantitativt olika resultat och baserat på behändighet borde den termiska tekniken av Sader et al. tillämpas. Vidare har det viktiga momentet att kalibrera fotodetektorn behandlats, och en ny teknik föreslås för att bestämma detektor-känsligheten genom att kombinera olika metoder. Slutligen beräknades en konverterings faktor, som gör det möjligt att utföra kalibrering av kantilevern i luft, men att själva friktionsmätningen sedan kan utföras i vätska.

Abstract [en]

In this thesis the atomic force microscope (AFM) and quartz crystal microbalance with dissipation (QCM-D) have been used to investigate interactions in bio-fibre model systems containing cellulose and xyloglucan (XG); a naturally occurring polysaccharide important for plant growth. In addition, the crucial element of friction force calibration has been studied to obtain accurate and quantitative results with the colloidal probe AFM.

Four different cellulose model surfaces with varying morphology have been evaluated using colloidal probe AFM. The normal surface forces for all the substrates studied were qualitatively similar. However, for a given surface roughness the adsorption of XG leads to a consistent decrease in friction coefficients for all substrates, suggesting that the effects on friction arising from either roughness or chemistry can be decoupled. To investigate the interaction between cellulose and XG exclusively the xyloglucan chains were enzymatically modified to include a thiol moiety at the chain end. These were further grafted to gold, forming a thiol-bonded xyloglucan brush-like layer. QCM-D experiments confirmed the graft to be biologically accessible to enzyme digestion using the plant enzyme endo-xyloglucanase TmNXG1. The friction coefficients obtained for the neat brush and the enzyme exposed substrate showed the same trend with surface roughness as for the cellulose surfaces. Adhesion measurements on this model surface indicated that the native specificity between xyloglucan and cellulose is retained.

A number of AFM cantilevers have been calibrated by different techniques to obtain both normal and frictional spring constants to evaluate the relative accuracy of the different methods. Good agreement was found between the techniques for obtaining the normal spring constant. Slightly higher deviations between the techniques used in obtaining the torsional spring constant were observed. However these deviations do not lead to quantitatively different results and based on convenience the thermal technique of Sader et al. is preferred. Further the important issue of the photodetector calibration is addressed and a new technique for obtaining the detector sensitivity by combining different methods is proposed. Finally a conversion factor was calculated that allows for the cantilever calibration to be done for example in air while actual friction measurements can be conducted in liquid.

Place, publisher, year, edition, pages
Stockholm: KTH, 2007. vi, 35 p.
Series
Trita-CHE-Report, ISSN 1654-1081 ; 1654-1081
Keyword
AFM, QCM-D, cellulose, xyloglucan, surface forces, friction, colloidal probe, nanotribology, biomimetic, enzymatic, polysaccharide, self assembly, grafting, thiol, spring constant, calibration, photodetector calibration.
National Category
Physical Chemistry
Identifiers
urn:nbn:se:kth:diva-4555 (URN)978-91-7178-796-5 (ISBN)
Presentation
2007-12-06, K1, Kemi, Teknikringen 56, Stockholm, 10:30
Opponent
Supervisors
Note
QC 20101115Available from: 2007-11-25 Created: 2007-11-25 Last updated: 2011-11-23Bibliographically approved
2. Interfacial Properties of Biomacromolecular Model Systems: Surface Forces and Nanotribology
Open this publication in new window or tab >>Interfacial Properties of Biomacromolecular Model Systems: Surface Forces and Nanotribology
2009 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

The nanotribology, adhesion and related interfacial properties of biomacromolecular systems have been studied.  The aim was to elucidate the role of physisorbed and chemically grafted bio-polymers implicated as mediators for cellulose based processing and material design.  To that end, model surfaces were prepared and characterized by the versatile techniques quartz crystal microbalance with dissipation (QCM-D) and atomic force microscopy (AFM) in colloidal probe mode.  A prerequisite for the latter in conducting quantifiable force and friction measurements lies in obtaining accurate values for the cantilever spring constants.  An investigation of various recently proposed calibration methods shows that they return essentially the same result, but that the route of Sader et al. is the least strenuous and indeed most reliable.  A novel approach for determining the required frictional detector sensitivity is proposed.

Cellulose model surfaces with varying morphology were evaluated.  For a given surface roughness the adsorption of xyloglucan, a nonionic polysaccharide, leads to a consistent decrease in the friction coefficients for all cellulose substrates, demonstrating that the effects on friction arising from either roughness or chemistry can be decoupled.  Moreover, xyloglucan grafts on gold show biological enzymatic accessibility, and their native affinity towards cellulose is retained, even in an extended brush conformation.

Chitosan, a cationic polysaccharide is also found to mediate lubrication and adhesion of cellulose in a solvent dependent manner, though the mechanisms are unlike those of xyloglucan.  At low pH the most efficient lubrication is achieved due to highly charged chitosan species extending out in the aqueous media, forming a highly hydrated cushion.  Conversely, at high pH the deswelling of the layer results in higher friction.  The same trend is observed between synthetic dual-responsive polyionic grafts on gold where the polymer charge is decisive for the friction properties. Above the lower critical solution temperature where the grafts are fully collapsed and display an attractive force, the friction is slightly reduced due to a nanoscopic flattening at the interface.

Finally, polymer grafts as matrix compatibilizers for bio-degradable cellulose based nano-composite applications were evaluated.  Adhesion is greatly promoted by chain entanglements.  The effect displays a dynamic diffusion based dependence of which the rate is significantly enhanced at a higher temperature close to the melting point of the polymeric layer.  No such adhesion benefit was obtained between ungrafted cellulose and the matrix material.

Abstract [sv]

Nanotribologin, adhesionen samt relaterade gränsskikts egenskaper av biomakromolekylära system har studerats.  Målet var att belysa inverkan av adsorberade samt kemiskt ympade bio-polymerer implicerade som medlare för cellulosa baserad förädling och material design.  För detta ändamål var modell ytor beredda och karakteriserade med de mångsidiga teknikerna kvarts kristall mikro våg med dissipation (QCM-D) och atom krafts mikroskopi (AFM) i kolloidal prob konfiguration.  En förutsättning för den senare i att utföra kvantifierbara kraft och friktionsmätningar ligger i att bestämma noggranna värden för kantilever-fjäderkonstanterna.  En undersökning av olika nyligen föreslagna kalibrerings metoder visar att de ger i huvudsak samma resultat, men att den av Sader et al. är minst krävande och sannerligen den mest tillförlitliga. Ett nytt tillvägagångsstätt för att bestämma den obligatoriska friktions detektor-känsligheten föreslås.

Cellulosa modell ytor med varierande morfologi utvärderades.   För en given ytråhet leder adsorption av xyloglukan, en icke-jonisk polysackarid, till en konsekvent reduktion av friktions-koefficienterna för alla substraten, vilket demonstrerar att effekten på friktion av antingen ytråhet eller kemi kan separeras.  Därtill visar sig xyloglukan ympningar på guld vara biologiskt enzymatiskt tillgängligt, och deras naturliga affinitet för cellulosa är bevarad, även i en utdragen borst-konformation.

Kitosan, en katjonisk polysackarid visar sig också förmedla smörjning och adhesion av cellulosa på ett lösnings beroende sätt, men mekanismerna är olika de för xyloglukan.  Vid lågt pH uppnås den mest effektiva smörjningen p. g. a. de högt laddade kitosankedjorna som sträcker ut sig i vatten lösningen och formar en högt hydratiserad dyna.  Omvänt, vid högt pH resulterar vattenhaltsminskningen av lagret i en högre friktion.  Samma tendens iakttas mellan syntetiskt dubbel-responsiva polyjoniska ympningar på guld där polymerladdningen är avgörande för friktionsegenskaperna.  Ovanför den lägre kritiska lösningstemperaturen där ympningen är helt kollapsad och uppvisar en attraktiv kraft är friktionen något reducerad        p. g. a. nanoskopisk utjämning vid gränsskiktet.

Slutligen, har polymerympningar som matris-kompatibiliterare för bio-nedbrytbara cellulosa baserade nano-komposit applikationer utvärderats.  Adhesionen är mycket gynnad av kedjeintrasslingar.  Effekten påvisar ett dynamiskt diffusionsbaserat beroende, av vilken takten är signifikant förhöjd vid en högre temperatur nära smältpunkten för polymerlagret.  Ingen sådan adhesionsfördel uppnåddes mellan den rena cellulosan och matrismaterialet.

Place, publisher, year, edition, pages
Stockholm: KTH, 2009. vii, 72 p.
Series
Trita-CHE-Report, ISSN 1654-1081 ; 2009:36
Keyword
afm, surface force, friction, composite material, model surface, quartz crystal microbalance, dissipation, cellulose, xyloglucan, chitosan, colloidal probe, nanotribology, biomimetic, enzymatic, polysaccharide, graft, fiber, thiol, spring constant, calibration, lubrication, polyion, responsive.
National Category
Physical Chemistry
Identifiers
urn:nbn:se:kth:diva-11002 (URN)978-91-7415-394-1 (ISBN)
Public defence
2009-09-25, FD5, AlbaNova Universitetscentrum, Roslagstullsbacken 21, Stockholm, 10:00 (English)
Opponent
Supervisors
Note
QC 20100804Available from: 2009-09-08 Created: 2009-09-03 Last updated: 2010-08-04Bibliographically approved
3. Interactions of cellulose and model surfaces
Open this publication in new window or tab >>Interactions of cellulose and model surfaces
2006 (English)Doctoral thesis, comprehensive summary (Other scientific)
Abstract [en]

The focus of this thesis is fundamental surface force and friction studies of silica and cellulose surfaces, performed mainly with the atomic force microscope (AFM). The normal interactions between model cellulose surfaces have been found to consist of a longer range double layer force with a short range steric interaction, the nature of which is extensively discussed. Both the surface charge and range of the steric force depend on the type of cellulose substrate used, as does the magnitude of the adhesion. Studies of friction on the same surfaces reveal that surface roughness is the determining factor for the friction coefficient, with which it increases monotonically. The absolute value, however, is determined by the surface chemistry.

The above is illustrated by studies of the effect of adsorbed xyloglucan, a prospective paper additive, which is found in the cell wall of all plants. Xyloglucan is like cellulose a poly- saccharide but the effect of its adsorption was to reduce the friction significantly, while following the identical trend with surface roughness. Xyloglucan also increases the adhesion between cellulose surfaces in a time dependent manner, interpreted in terms of a diffusive bridging interaction. These facts combined provide a mechanistic explanation to contemporaneous findings about xyloglucans benefit in paper strength and formation.

In air, the adhesion between e.g. particles or fibres, must be at least partially determined by the formation of capillary condensates. The dependence of capillary condensation on relative humidity is however not yet fully understood so studies have been performed to cast light on this phenomenon. Above about 60 % relative humidity the adhesion and friction increase dramatically due to the formation of large capillary condensates. The extent of the condensates depends both on the time the surfaces equilibrate, but also on the surface roughness. Harvesting of the condensate during shearing is also observed through hysteresis of the friction-load relationship.

Measurements of surface forces and friction in surfactant systems show a clear relation between the adsorbed surfactant layer and the barrier force and adhesion, which in turn determine the friction. All of these interactions are critically dependent on the composition of the surfactant solution. A mixed surfactant system has been studied consisting of a trimethylammonium cationic surfactant and a polyoxyethylene nonionic surfactant. The results are interpreted in terms of current theories of adsorption and synergistic interactions. Finally, a novel technique for the in situ calibration and measurement of friction with the AFM is proposed. Comparison with lateral measurements show that the approach is successful.

Place, publisher, year, edition, pages
Stockholm: KTH, 2006. 58 p.
Series
Trita-YTK, ISSN 1650-0490 ; 0603
National Category
Physical Chemistry
Identifiers
urn:nbn:se:kth:diva-619 (URN)91-7178-260-5 (ISBN)
Public defence
2006-02-24, sal F3, Lindstedtsvägen 26, Stockholm, 10:00
Opponent
Supervisors
Note
QC 20100920Available from: 2006-02-10 Created: 2006-02-10 Last updated: 2011-12-19Bibliographically approved

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