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Pilkington, G. A., Harris, K., Bergendal, E., Reddy, A. B., Palsson, G. K., Vorobiev, A., . . . Rutland, M. W. (2018). Electro-responsivity of ionic liquid boundary layers in a polar solvent revealed by neutron reflectance. Journal of Chemical Physics, 148(19), Article ID 193806.
Open this publication in new window or tab >>Electro-responsivity of ionic liquid boundary layers in a polar solvent revealed by neutron reflectance
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2018 (English)In: Journal of Chemical Physics, ISSN 0021-9606, E-ISSN 1089-7690, Vol. 148, no 19, article id 193806Article in journal (Refereed) Published
Abstract [en]

Using neutron reflectivity, the electro-responsive structuring of the non-halogenated ionic liquid (IL) trihexyl(tetradecyl)phosphonium-bis(mandelato)borate, [P6,6,6,14][BMB], has been studied at a gold electrode surface in a polar solvent. For a 20% w/w IL mixture, contrast matched to the gold surface, distinct Kiessig fringes were observed for all potentials studied, indicative of a boundary layer of different composition to that of the bulk IL-solvent mixture. With applied potential, the amplitudes of the fringes from the gold-boundary layer interface varied systematically. These changes are attributable to the differing ratios of cations and anions in the boundary layer, leading to a greater or diminished contrast with the gold electrode, depending on the individual ion scattering length densities. Such electro-responsive changes were also evident in the reflectivities measured for the pure IL and a less concentrated (5% w/w) IL-solvent mixture at the same applied potentials, but gave rise to less pronounced changes. These measurements, therefore, demonstrate the enhanced sensitivity achieved by contrast matching the bulk solution and that the structure of the IL boundary layers formed in mixtures is strongly influenced by the bulk concentration. Together these results represent an important step in characterising IL boundary layers in IL-solvent mixtures and provide clear evidence of electro-responsive structuring of IL ions in their solutions with applied potential.

Keywords
Electrodes, Gold, Ionic liquids, Ions, Mixtures, Reflection, Solvents, Applied potentials, Bulk concentration, Contrast matching, Enhanced sensitivity, Liquid boundary layers, Neutron reflectance, Neutron reflectivity, Solvent mixtures, Boundary layers
National Category
Natural Sciences
Identifiers
urn:nbn:se:ri:diva-33422 (URN)10.1063/1.5001551 (DOI)2-s2.0-85041289749 (Scopus ID)
Available from: 2018-03-09 Created: 2018-03-09 Last updated: 2018-08-17Bibliographically approved
Shah, F. U., Holmgren, A., Rutland, M. W., Glavatskih, S. & Antzutkin, O. (2018). Interfacial Behavior of Orthoborate Ionic Liquids at Inorganic Oxide Surfaces Probed by NMR, IR, and Raman Spectroscopy. The Journal of Physical Chemistry C, 122(34), 19687-19698
Open this publication in new window or tab >>Interfacial Behavior of Orthoborate Ionic Liquids at Inorganic Oxide Surfaces Probed by NMR, IR, and Raman Spectroscopy
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2018 (English)In: The Journal of Physical Chemistry C, ISSN 1932-7447, E-ISSN 1932-7455, Vol. 122, no 34, p. 19687-19698Article in journal (Refereed) Published
Abstract [en]

Absorption modes and the reactivity of nonhalogenated ionic liquids (ILs) at inorganic oxide surfaces of γ-Al2O3, MgO, and SiO2 particles were characterized using multinuclear (11B, 31P, and 29Si) solid-state magic-angle-spinning NMR, FTIR, and Raman spectroscopy. ILs are composed of the trihexyl(tetradecyl)phosphonium cation, [P6,6,6,14]+, and bis(mandelato)borate, [BMB]-, or bis(salicylato)borate, [BScB]-, anions. Spectroscopic measurements were performed on room-temperature (298 K) samples and samples exposed to 15 h at 373 K. The single-pulse 11B NMR data of heated [P6,6,6,14][BMB] mixed with the inorganic oxides showed a significant change in the spectra of the anion for all three oxides. In contrast, no such spectral changes were detected for heated [P6,6,6,14][BScB] mixed with the inorganic oxides. 31P MAS NMR data for the IL/metal oxide systems revealed interactions between [P6,6,6,14]+ and the surfaces of oxides. A significant intensity of 31P CP-MAS NMR signals indicated a low mobility of cations in these systems. The existence of strongly adhered surface layers of ILs on SiO2 particles was also confirmed by 1H-29Si CP-MAS NMR spectroscopy. FTIR and Raman spectroscopic data revealed strong interactions between the anions and the inorganic surfaces, and there is a strong correlation with the data obtained from NMR spectroscopy. Although their chemical structures are rather similar, the [BScB]- anion is more stable than the [BMB]- anion at the inorganic oxide surfaces.

Keywords
Alumina, Aluminum oxide, Ionic liquids, Magic angle spinning, Magnesia, Negative ions, Nuclear magnetic resonance spectroscopy, Positive ions, Raman spectroscopy, Silica, Inorganic surfaces, Interfacial behaviors, Ionic liquid (ils), IR and Raman spectroscopy, Phosphonium cations, Solid state magic angle spinning NMR, Spectroscopic measurements, Strong interaction, Fourier transform infrared spectroscopy
National Category
Natural Sciences
Identifiers
urn:nbn:se:ri:diva-35645 (URN)10.1021/acs.jpcc.8b06049 (DOI)2-s2.0-85052316588 (Scopus ID)
Note

Funding details: LTU, Luther Theological University; Funding details: 621-2013-5171, VR, Vetenskapsrådet; Funding details: 621-2014-4694, VR, Vetenskapsrådet; Funding details: KAW2012.0078, Knut och Alice Wallenbergs Stiftelse; Funding text: The Knut and Alice Wallenberg Foundation (project number KAW2012.0078), Swedish Research Council (projects numbers 621-2013-5171 (O.N.A. and F.U.S.) and 621-2014-4694 (S.G

Available from: 2018-11-06 Created: 2018-11-06 Last updated: 2018-11-06Bibliographically approved
Skedung, L., El Rawadi, C., Arvidsson, M., Farcet, C., Luengo, G. S., Breton, L. & Rutland, M. W. (2018). Mechanisms of tactile sensory deterioration amongst the elderly. Scientific Reports, 8(1), Article ID 5303.
Open this publication in new window or tab >>Mechanisms of tactile sensory deterioration amongst the elderly
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2018 (English)In: Scientific Reports, ISSN 2045-2322, E-ISSN 2045-2322, Vol. 8, no 1, article id 5303Article in journal (Refereed) Published
Abstract [en]

It is known that roughness-smoothness, hardness-softness, stickiness-slipperiness and warm-cold are predominant perceptual dimensions in macro-, micro- and nano- texture perception. However, it is not clear to what extent active tactile texture discrimination remains intact with age. The general decrease in tactile ability induces physical and emotional dysfunction in elderly, and has increasing significance for an aging population. We report a method to quantify tactile acuity based on blinded active exploration of systematically varying micro-textured surfaces and a same-different paradigm. It reveals that elderly participants show significantly reduced fine texture discrimination ability. The elderly group also displays statistically lower finger friction coefficient, moisture and elasticity, suggesting a link. However, a subpopulation of the elderly retains discrimination ability irrespective of cutaneous condition and this can be related to a higher density of somatosensory receptors on the finger pads. Skin tribology is thus not the primary reason for decline of tactile discrimination with age. The remediation of cutaneous properties through rehydration, however leads to a significantly improved tactile acuity. This indicates unambiguously that neurological tactile loss can be temporarily compensated by restoring the cutaneous contact mechanics. Such mechanical restoration of tactile ability has the potential to increase the quality of life in elderly. 

Keywords
aged, article, controlled study, deterioration, elasticity, finger, friction, human, moisture, quality of life, rehydration, skin, tactile discrimination
National Category
Natural Sciences
Identifiers
urn:nbn:se:ri:diva-33788 (URN)10.1038/s41598-018-23688-6 (DOI)2-s2.0-85045892223 (Scopus ID)
Available from: 2018-05-03 Created: 2018-05-03 Last updated: 2018-08-17Bibliographically approved
Badal Tejedor, M., Pazesh, S., Nordgren, N., Schuleit, M., Rutland, M. W., Alderborn, G. & Millqvist-Fureby, A. (2018). Milling induced amorphisation and recrystallization of α-lactose monohydrate. International Journal of Pharmaceutics, 537(1-2), 140-147
Open this publication in new window or tab >>Milling induced amorphisation and recrystallization of α-lactose monohydrate
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2018 (English)In: International Journal of Pharmaceutics, ISSN 0378-5173, E-ISSN 1873-3476, Vol. 537, no 1-2, p. 140-147Article in journal (Refereed) Published
Abstract [en]

Preprocessing of pharmaceutical powders is a common procedure to condition the materials for a better manufacturing performance. However, such operations may induce undesired material properties modifications when conditioning particle size through milling, for example. Modification of both surface and bulk material structure will change the material properties, thus affecting the processability of the powder. Hence it is essential to control the material transformations that occur during milling. Topographical and mechanical changes in surface properties can be a preliminary indication of further material transformations. Therefore a surface evaluation of the α-lactose monohydrate after short and prolonged milling times has been performed. Unprocessed α-lactose monohydrate and spray dried lactose were evaluated in parallel to the milled samples as reference examples of the crystalline and amorphous lactose structure. Morphological differences between unprocessed α-lactose, 1 h and 20 h milled lactose and spray dried lactose were detected from SEM and AFM images. Additionally, AFM was used to simultaneously characterize particle surface amorphicity by measuring energy dissipation. Extensive surface amorphicity was detected after 1 h of milling while prolonged milling times showed only a moderate particle surface amorphisation. Bulk material characterization performed with DSC indicated a partial amorphicity for the 1 h milled lactose and a fully amorphous thermal profile for the 20 h milled lactose. The temperature profiles however, were shifted somewhat in the comparison to the amorphous reference, particularly after extended milling, suggesting a different amorphous state compared to the spray-dried material. Water loss during milling was measured with TGA, showing lower water content for the lactose amorphized through milling compared to spray dried amorphous lactose. The combined results suggest a surface-bulk propagation of the amorphicity during milling in combination with a different amorphous structural conformation to that of the amorphous spray dried lactose. The hardened surface may be due to either surface crystallization of lactose or to formation of a low-water glass transition.

Keywords
Amorphisation, Atomic force microscopy, Differential scanning calorimetry, Lactose, Mechanical properties, Milling, Recrystallization, Tableting, TGA, alpha lactose, Article, conformation, crystallization, energy, glass transition temperature, morphology, particle size, powder, priority journal, scanning electron microscopy, spray drying, surface property, thermogravimetry
National Category
Natural Sciences
Identifiers
urn:nbn:se:ri:diva-33233 (URN)10.1016/j.ijpharm.2017.12.021 (DOI)2-s2.0-85038844261 (Scopus ID)
Available from: 2018-02-13 Created: 2018-02-13 Last updated: 2018-08-17Bibliographically approved
Besharat, Z., Yazdi, M. G., Wakeham, D., Johnson, M., Rutland, M. W., Gothelid, M. & Gronbeck, H. (2018). Se-C Cleavage of Hexane Selenol at Steps on Au(111). Langmuir, 34(8), 2630-2636
Open this publication in new window or tab >>Se-C Cleavage of Hexane Selenol at Steps on Au(111)
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2018 (English)In: Langmuir, ISSN 0743-7463, E-ISSN 1520-5827, Vol. 34, no 8, p. 2630-2636Article in journal (Refereed) Published
Abstract [en]

Selenols are considered as an alternative to thiols in self-assembled monolayers, but the Se-C bond is one limiting factor for their usefulness. In this study, we address the stability of the Se-C bond by a combined experimental and theoretical investigation of gas phase-deposited hexane selenol (CH3(CH2)(5)SeH) on Au(111) using photoelectron spectroscopy, scanning tunneling microscopy, and density functional theory (DFT). Experimentally, we find that initial adsorption leaves atomic Se on the surface without any carbon left on the surface, whereas further adsorption generates a saturated selenolate layer. The Se 3d component from atomic Se appears at 0.85 eV lower binding energy than the selenolate-related component. DFT calculations show that the most stable structure of selenols on Au(111) is in the form of RSe-Au-SeR complexes adsorbed on the unreconstructed Au(111) surface. This is similar to thiols on Au(111). Calculated Se 3d core-level shifts between elemental Se and selenolate in this structure nicely reproduce the experimentally recorded shifts. Dissociation of RSeH and subsequent formation of RH are found to proceed with high barriers on defect-free Au(111) terraces, with the highest barrier for scissoring R-Se. However, at steps, these barriers are considerably lower, allowing for Se-C bond breaking and hexane desorption, leaving elemental Se at the surface. Hexane is the selenol to selenolate formed by replacing the Se-C bond with a H-C bond by using the hydrogen liberated from transformation.

National Category
Natural Sciences
Identifiers
urn:nbn:se:ri:diva-33712 (URN)10.1021/acs.langmuir.7b03713 (DOI)2-s2.0-85042636157 (Scopus ID)
Available from: 2018-04-14 Created: 2018-04-14 Last updated: 2019-01-10Bibliographically approved
Badal Tejedor, M., Nordgren, N., Schuleit, M., Millqvist-Fureby, A. & Rutland, M. W. (2017). AFM Colloidal Probe Measurements Implicate Capillary Condensation in Punch-Particle Surface Interactions during Tableting. Langmuir, 33(46), 13180-13188
Open this publication in new window or tab >>AFM Colloidal Probe Measurements Implicate Capillary Condensation in Punch-Particle Surface Interactions during Tableting
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2017 (English)In: Langmuir, ISSN 0743-7463, E-ISSN 1520-5827, Vol. 33, no 46, p. 13180-13188Article in journal (Refereed) Published
Abstract [en]

Adhesion of the powders to the punches is a common issue during tableting. This phenomenon is known as sticking and affects the quality of the manufactured tablets. Defective tablets increase the cost of the manufacturing process. Thus, the ability to predict the tableting performance of the formulation blend before the process is scaled-up is important. The adhesive propensity of the powder to the tableting tools is mostly governed by the surface-surface adhesive interactions. Atomic force microscopy (AFM) colloidal probe is a surface characterization technique that allows the measurement of the adhesive interactions between two materials of interest. In this study, AFM steel colloidal probe measurements were performed on ibuprofen, MCC (microcrystalline cellulose), α-lactose monohydrate, and spray-dried lactose particles as an approach to modeling the punch-particle surface interactions during tableting. The excipients (lactose and MCC) showed constant, small, attractive, and adhesive forces toward the steel surface after a repeated number of contacts. In comparison, ibuprofen displayed a much larger attractive and adhesive interaction increasing over time both in magnitude and in jump-in/jump-out separation distance. The type of interaction acting on the excipient-steel interface can be related to a van der Waals force, which is relatively weak and short-ranged. By contrast, the ibuprofen-steel interaction is described by a capillary force profile. Even though ibuprofen is not highly hydrophilic, the relatively smooth surfaces of the crystals allow "contact flooding" upon contact with the steel probe. Capillary forces increase because of the "harvesting" of moisture - due to the fast condensation kinetics - leaving a residual condensate that contributes to increase the interaction force after each consecutive contact. Local asperity contacts on the more hydrophilic surface of the excipients prevent the flooding of the contact zone, and there is no such adhesive effect under the same ambient conditions. The markedly different behavior detected by force measurements clearly shows the sticky and nonsticky propensity of the materials and allows a mechanistic description.

Keywords
Atomic force microscopy, Cellulose, Characterization, Condensation, Floods, Hydrophilicity, Probes, Sugars, Van der Waals forces, Adhesive interaction, Alpha lactose monohydrate, Capillary condensation, Condensation kinetics, Hydrophilic surfaces, Manufacturing process, Micro-crystalline cellulose, Surface characterization, Drug products
National Category
Natural Sciences
Identifiers
urn:nbn:se:ri:diva-33146 (URN)10.1021/acs.langmuir.7b02189 (DOI)2-s2.0-85034836128 (Scopus ID)
Available from: 2018-01-31 Created: 2018-01-31 Last updated: 2018-08-17Bibliographically approved
Li, H., Rutland, M. W., Watanabe, M. & Atkin, R. (2017). Boundary layer friction of solvate ionic liquids as a function of potential. Faraday discussions (Online), 199, 311-322
Open this publication in new window or tab >>Boundary layer friction of solvate ionic liquids as a function of potential
2017 (English)In: Faraday discussions (Online), ISSN 1359-6640, E-ISSN 1364-5498, Vol. 199, p. 311-322Article in journal (Refereed) Published
Abstract [en]

Atomic force microscopy (AFM) has been used to investigate the potential dependent boundary layer friction at solvate ionic liquid (SIL)-highly ordered pyrolytic graphite (HOPG) and SIL-Au(111) interfaces. Friction trace and retrace loops of lithium tetraglyme bis(trifluoromethylsulfonyl)amide (Li(G4) TFSI) at HOPG present clearer stick-slip events at negative potentials than at positive potentials, indicating that a Li+ cation layer adsorbed to the HOPG lattice at negative potentials which enhances stick-slip events. The boundary layer friction data for Li(G4) TFSI shows that at HOPG, friction forces at all potentials are low. The TFSI- anion rich boundary layer at positive potentials is more lubricating than the Li+ cation rich boundary layer at negative potentials. These results suggest that boundary layers at all potentials are smooth and energy is predominantly dissipated via stick-slip events. In contrast, friction at Au(111) for Li(G4) TFSI is significantly higher at positive potentials than at negative potentials, which is comparable to that at HOPG at the same potential. The similarity of boundary layer friction at negatively charged HOPG and Au(111) surfaces indicates that the boundary layer compositions are similar and rich in Li+ cations for both surfaces at negative potentials. However, at Au(111), the TFSI- rich boundary layer is less lubricating than the Li+ rich boundary layer, which implies that anion reorientations rather than stick-slip events are the predominant energy dissipation pathways. This is confirmed by the boundary friction of Li(G4) NO3 at Au(111), which shows similar friction to Li(G4) TFSI at negative potentials due to the same cation rich boundary layer composition, but even higher friction at positive potentials, due to higher energy dissipation in the NO3 - rich boundary layer. © The Royal Society of Chemistry.

National Category
Natural Sciences
Identifiers
urn:nbn:se:ri:diva-31135 (URN)10.1039/c6fd00236f (DOI)2-s2.0-85024131651 (Scopus ID)
Available from: 2017-08-25 Created: 2017-08-25 Last updated: 2019-01-03Bibliographically approved
Rutland, M. W. (2017). Chemical physics of electroactive materials: Concluding remarks. Faraday discussions (Online), 199, 615-630
Open this publication in new window or tab >>Chemical physics of electroactive materials: Concluding remarks
2017 (English)In: Faraday discussions (Online), ISSN 1359-6640, E-ISSN 1364-5498, Vol. 199, p. 615-630Article in journal (Refereed) Published
Abstract [en]

It is an honour to be charged with providing the concluding remarks for a Faraday Discussion. As many have remarked before, it is nonetheless a prodigious task, and what follows is necessarily a personal, and probably perverse, view of a watershed event in the Chemical Physics of Electroactive materials. The spirit of the conference was captured in a single sentence during the meeting itself. "It is the nexus between rheology, electrochemistry, colloid science and energy storage". The current scientific climate is increasingly dominated by a limited number of global challenges, and there is thus a tendency for research to resemble a football match played by 6 year olds, where everyone on the field chases the (funding) ball instead of playing to their "discipline". It is thus reassuring to see how the application of rigorous chemical physics is leading to ingenious new solutions for both energy storage and harvesting, via, for example, nanoactuation, electrowetting, ionic materials and nanoplasmonics. In fact, the same language of chemical physics allows seamless transition between applications as diverse as mechano-electric energy generation, active moisture transport and plasmonic shutters-even the origins of life were addressed in the context of electro-autocatalysis!.

National Category
Natural Sciences
Identifiers
urn:nbn:se:ri:diva-31179 (URN)10.1039/c7fd00176b (DOI)2-s2.0-85024122602 (Scopus ID)
Available from: 2017-08-23 Created: 2017-08-23 Last updated: 2018-08-17Bibliographically approved
Badal Tejedor, M., Nordgren, N., Schuleit, M., Pazesh, S., Alderborn, G., Millqvist-Fureby, A. & Rutland, M. W. (2017). Determination of interfacial amorphicity in functional powders. Langmuir, 33(4), 920-926
Open this publication in new window or tab >>Determination of interfacial amorphicity in functional powders
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2017 (English)In: Langmuir, ISSN 0743-7463, E-ISSN 1520-5827, Vol. 33, no 4, p. 920-926Article in journal (Refereed) Published
Abstract [en]

The nature of the surfaces of particles of pharmaceutical ingredients, food powders, and polymers is a determining factor for their performance in for example tableting, powder handling, or mixing. Changes on the surface structure of the material will impact the flow properties, dissolution rate, and tabletability of the powder blend. For crystalline materials, surface amorphization is a phenomenon which is known to impact performance. Since it is important to measure and control the level of amorphicity, several characterization techniques are available to determine the bulk amorphous content of a processed material. The possibility of characterizing the degree of amorphicity at the surface, for example by studying the mechanical properties of the particles' surface at the nanoscale, is currently only offered by atomic force microscopy (AFM). The AFM PeakForce QNM technique has been used to measure the variation in energy dissipation (eV) at the surface of the particles which sheds light on the mechanical changes occurring as a result of amorphization or recrystallization events. Two novel approaches for the characterization of amorphicity are presented here. First, since particles are heterogeneous, we present a methodology to present the results of extensive QNM analysis of multiple particles in a coherent and easily interpreted manner, by studying cumulative distributions of dissipation data with respect to a threshold value which can be used to distinguish the crystalline and amorphous states. To exemplify the approach, which is generally applicable to any material, reference materials of purely crystalline α-lactose monohydrate and completely amorphous spray dried lactose particles were compared to a partially amorphized α-lactose monohydrate sample. Dissipation data are compared to evaluations of the lactose samples with conventional AFM and SEM showing significant topographical differences. Finally, the recrystallization of the surface amorphous regions in response to humidity was followed by studying the dissipation response of a well-defined surface region over time, which confirms both that dissipation measurement is a useful measure of surface amorphicity and that significant recrystallization occurs at the surface in response to humidity.

National Category
Chemical Sciences
Identifiers
urn:nbn:se:ri:diva-28201 (URN)10.1021/acs.langmuir.6b03969 (DOI)2-s2.0-85011117083 (Scopus ID)
Available from: 2017-04-03 Created: 2017-04-03 Last updated: 2018-08-17Bibliographically approved
Arvidsson, M., Ringstad, L., Skedung, L., Duvefelt, K. & Rutland, M. W. (2017). Feeling fine - the effect of topography and friction on perceived roughness and slipperiness. Biotribology, 11, 92-101
Open this publication in new window or tab >>Feeling fine - the effect of topography and friction on perceived roughness and slipperiness
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2017 (English)In: Biotribology, ISSN 2352-5738, Vol. 11, p. 92-101Article in journal (Refereed) Published
Abstract [en]

(1) Background. To design materials with specific haptic qualities, it is important to understand both the contribution of physical attributes from the surfaces of the materials and the perceptions that are involved in the haptic interaction. (2) Methods. A series of 16 wrinkled surfaces consisting of two similar materials of different elastic modulus and 8 different wrinkle wavelengths were characterized in terms of surface roughness and tactile friction coefficient. Sixteen participants scaled the perceived Roughness and Slipperiness of the surfaces using free magnitude estimation. Friction experiments were performed both by participants and by a trained experimenter with higher control. (3) Results and discussion. The trends in friction properties were similar for the group of participants performing the friction measurements in an uncontrolled way and the experiments performed under well-defined conditions, showing that the latter type of measurements represent the general friction properties well. The results point to slipperiness as the key perception dimension for textures below 100. μm and roughness above 100. μm. Furthermore, it is apparent that roughness and slipperiness perception of these types of structures are not independent. The friction is related to contact area between finger and material. Somewhat surprising was that the material with the higher elastic modulus was perceived as more slippery. A concluding finding was that the flat (high friction) reference surfaces were scaled as rough, supporting the theory that perceived roughness itself is a multidimensional construct with both surface roughness and friction component.

Keywords
Friction, Roughness, Slipperiness, Tactile perception
National Category
Natural Sciences
Identifiers
urn:nbn:se:ri:diva-31183 (URN)10.1016/j.biotri.2017.01.002 (DOI)2-s2.0-85023162786 (Scopus ID)
Note

Export Date: 23 August 2017; Article in Press

Available from: 2017-08-23 Created: 2017-08-23 Last updated: 2018-08-17Bibliographically approved
Identifiers
ORCID iD: ORCID iD iconorcid.org/0000-0002-8935-8070

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