Experimental Investigation of the Velocity Effect on Adhesion Forces with an Atomic Force Microscope Atomic Force Microscope

Capillary forces are significantly dominant in adhesive forces measured with an atomic force microscope (AFM) in ambient air, which are always thought to be dependent on water film thickness, relative humidity, and the free energy of water film. We study the nature of the pull-off force on a variety of surfaces as a function of tip velocity. It is found that the capillary forces are of relatively strong dependence on tip velocity. The present experiment is expected to provide a better understanding of the work mechanism of AFM in ambient air.

Molecular Dynamics Simulation Of Adhesion Forces In A Dipalmitoylphosphatidylcholine Membrane

Adhesion forces of Dipalmitoylphosphatidylcholine ( DPPC) membrane in the gel phase are investigated by molecular dynamics ( MD) simulation. In the simulations, individual DPPC molecules are pulled out of DPPC membranes with different rates and we get the maximum adhesion forces of DPPC membrane. We find that the maximum adhesion forces increase with pull rate, from about 400 to 700 pN when pull rates are from 0.001 to 0.03 nm/ps. We analyze the relationship between pull rate and adhesion forces of different origins using Brownian dynamics and notice that viscosity of solvent plays an important role in adhesion forces. Then we simulate the motion of a single DPPC molecule in solvent and it elucidates that the maximum drag force is almost linear with respect to the pull rate. We use Stokes' relation to describe the motion of a single DPPC molecule and deduce the effective length of a DPPC molecule. Conformational analyses indicate that the free energy variation of a DPPC molecule inside and outside of the DPPC membrane is an essential part of adhesion energy.

Molecular dynamics simulation of adhesion forces in a dipalmitoylphosphatidylcholine membrane

Adhesion forces of Dipalmitoylphosphatidylcholine ( DPPC) membrane in the gel phase are investigated by molecular dynamics ( MD) simulation. In the simulations, individual DPPC molecules are pulled out of DPPC membranes with different rates and we get the maximum adhesion forces of DPPC membrane. We find that the maximum adhesion forces increase with pull rate, from about 400 to 700 pN when pull rates are from 0.001 to 0.03 nm/ps. We analyze the relationship between pull rate and adhesion forces of different origins using Brownian dynamics and notice that viscosity of solvent plays an important role in adhesion forces. Then we simulate the motion of a single DPPC molecule in solvent and it elucidates that the maximum drag force is almost linear with respect to the pull rate. We use Stokes' relation to describe the motion of a single DPPC molecule and deduce the effective length of a DPPC molecule. Conformational analyses indicate that the free energy variation of a DPPC molecule inside and outside of the DPPC membrane is an essential part of adhesion energy.

Mapping of adhesion forces on soil minerals in air and water by atomic force spectroscopy (AFS)

The adhesion force between an atomic force microscope (AFM) tip and sample surfaces, mica and quartz substrates, was measured in air and water. The force curves show that the adhesion has a strong dependence on both the surface roughness and the environmental conditions surrounding the sample. The variability of the adhesion force was examined in a series of measurements taken at the same point, as well as at different places on the sample surface. The adhesion maps obtained from the distribution of the measured forces indicated regions contaminated by either organic compounds or adsorbed water. Using simple mathematical expressions we could quantitatively predict the adhesion force behavior in both air and water. The experimental results are in good agreement with theoretical calculations, where the adhesion forces in air and water were mostly associated with capillary and van der Waals forces, respectively. A small long-range repulsive force is also observed in water due to the overlapping electrical double-layers formed on both the tip and sample surfaces.

Development of a system measuring adhesion forces in powder collectives

Fine powders commonly have poor flowability and dispersibility due to interparticle adhesion that leads to formation of agglomerates. Knowing about adhesion in particle collectives is indispensable to gain a deeper fundamental understanding of particle behavior in powders. Especially in pharmaceutical industry a control of adhesion forces in powders is mandatory to improve the performance of inhalation products. Typically the size of inhalable particles is in the range of 1 - 5 µm. In this thesis, a new method was developed to measure adhesion forces of particles as an alternative to the established colloidal probe and centrifuge technique, which are both experimentally demanding, time consuming and of limited practical applicability. The new method is based on detachment of individual particles from a surface due to their inertia. The required acceleration in the order of 500 000 g is provided by a Hopkinson bar shock excitation system and measured via laser vibrometry. Particle detachment events are detected on-line by optical video microscopy. Subsequent automated data evaluation allows obtaining a statistical distribution of particle adhesion forces. To validate the new method, adhesion forces for ensembles of single polystyrene and silica microspheres on a polystyrene coated steel surface were measured under ambient conditions. It was possible to investigate more than 150 individual particles in one experiment and obtain adhesion values of particles in a diameter range of 3 - 13 µm. This enables a statistical evaluation while measuring effort and time are considerably lower compared to the established techniques. Measured adhesion forces of smaller particles agreed well with values from colloidal probe measurements and theoretical predictions. However, for the larger particles a stronger increase of adhesion with diameter was observed. This discrepancy might be induced by surface roughness and heterogeneity that influence small and large particles differently. By measuring adhesion forces of corrugated dextran particles with sizes down to 2 µm it was demonstrated that the Hopkinson bar method can be used to characterize more complex sample systems as well. Thus, the new device will be applicable to study a broad variety of different particle-surface combinations on a routine basis, including strongly cohesive powders like pharmaceutical drugs for inhalation.

The differential adhesion forces of anterior cruciate and medial collateral ligament fibroblasts: effects of tropomodulin, talin, vinculin, and alpha-actinin.

We have determined the effects of tropomodulin (Tmod), talin, vinculin, and alpha-actinin on ligament fibroblast adhesion. The anterior cruciate ligament (ACL), which lacks a functional healing response, and the medial collateral ligament (MCL), a functionally healing ligament, were selected for this study. The micropipette aspiration technique was used to determine the forces needed to separate ACL and MCL cells from a fibronectin-coated surface. Delivery of exogenous tropomodulin, an actin-filament capping protein, into MCL fibroblasts significantly increased adhesion, whereas its monoclonal antibody (mAb) significantly decreased cell adhesiveness. However, for ACL fibroblasts, Tmod significantly reduced adhesion, whereas its mAb had no effect. mAbs to talin, vinculin, and alpha-actinin significantly decreased the adhesion of both ACL and MCL cells with increasing concentrations of antibody, and also reduced stress fiber formation and cell spreading rate as revealed by immunofluorescence microscopy. Disruption of actin filament and microtubule assembly with cytochalasin D and colchicine, respectively, also significantly reduced adhesion in ACL and MCL cells. In conclusion, both ACL and MCL fibroblast adhesion depends on cytoskeletal assembly; however, this dependence differs between ACL and MCL fibroblasts in many ways, especially in the role of Tmod. These results add yet another possible factor in explaining the clinical differences in healing between the ACL and the MCL.

Theoretical Models for Surface Forces and Adhesion and Their Measurement Using Atomic Force Microscopy

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Adhesion and dispersion of salmeterol xinofoate from lactose interactive mixtures for inhalation - can surface roughness of carriers determine performance

The objective was to understand the influence of the surface roughness of lactose carriers on the adhesion and dispersion of salmeterol xinafoate (SX) from interactive mixtures. The surface roughness of lactose carriers was determined by confocal microscopy. Particle images and adhesion forces between SX and lactose particles were determined by Atomic Force Microscopy. The dispersion of SX (2.5%) from interactive mixtures with lactose was determined using a twin-stage impinger (TSI) with a Rotahaler® at an airflow rate of 60L/min. SX was analysed using a validated HPLC assay. The RMS Rq of lactose carriers ranged from 0.93-2.84μm, the Fine Particle Fraction (FPF) of SX ranged between 4 and 24 percent and average adhesion force between a SX and lactose particles ranged between 49 and 134 nN. No direct correlation was observed between the RMS Rq of lactose carriers and either the FPF of SX for the interactive mixtures or the adhesion force of a SX on the lactose particles; however, the presence of fine lactose associated with the carrier surface increased the FPF of SX. Dispersion through direct SX detachment from the carrier surface was not consistent with the poor correlations described and was more likely to occur through complex particulate interactions involving fine lactose.

Colloidal drug probe : method development and validation for adhesion force measurement using atomic force microscopy

This study demonstrates a novel technique of preparing drug colloid probes to determine the adhesion force between the drug salbutamol sulphate (SS) and the surfaces of polymer microparticles to be used as carriers for the dispersion of drug particles from a dry powder inhaler (DPI) formulation. Initially model silica probes of approximately 4 μm size, similar to a drug particle used in DPI formulations, were coated with a saturated SS solution with the aid of capillary forces acting between the silica probe and the drug solution. The developed method of ensuring a smooth and uniform layer of SS on the silica probe was validated using X-Ray Photoelectron Spectroscopy (XPS) and Scanning Electron Microscopy (SEM). Using the same technique, silica microspheres preattached on the AFM cantilever were coated with SS. The adhesion forces between the silica probe and drug coated silica (drug probe) and polymer surfaces (hydrophilic and hydrophobic) were determined. Our experimental results showed that the technique for preparing the drug probe was robust and can be used to determine the adhesion force between hydrophilic/hydrophobic drug probe and carrier surfaces to gain a better understanding on drug carrier adhesion forces in DPI formulations.

Colloidal drug probe : Method development and validation for adhesion force measurement using Atomic Force Microscopy

This study demonstrates a novel technique of preparing drug colloid probes to determine the adhesion force between a model drug salbutamol sulphate (SS) and the surfaces of polymer microparticles to be used as carriers for the dispersion of drug particles from dry powder inhaler (DPI) formulations. Model silica probes of approximately 4 lm size, similar to a drug particle used in DPI formulations, were coated with a saturated SS solution with the aid of capillary forces acting between the silica probe and the drug solution. The developed method of ensuring a smooth and uniform layer of SS on the silica probe was validated using X-ray Photoelectron Spectroscopy (XPS) and Scanning Electron Microscopy (SEM). Using the same technique, silica microspheres pre-attached on the AFM cantilever were coated with SS. The adhesion forces between the silica probe and drug coated silica (drug probe) and polymer surfaces (hydrophilic and hydrophobic) were determined. Our experimental results showed that the technique for preparing the drug probe was robust and can be used to determine the adhesion force between hydrophilic/ hydrophobic drug probe and carrier surfaces to gain a better understanding on drug carrier adhesion forces in DPI formulations.

Design and control of a climbing robot based on hot melt adhesion

Robust climbing in unstructured environments has been one of the long-standing challenges in robotics research. Among others, the control of large adhesion forces is still an important problem that significantly restricts the locomotion performance of climbing robots. The main contribution of this paper is to propose a novel approach to autonomous robot climbing which makes use of hot melt adhesion (HMA). The HMA material is known as an economical solution to achieve large adhesion forces, which can be varied by controlling the material temperature. For locomotion on both inclined and vertical walls, this paper investigates the basic characteristics of HMA material, and proposes a design and control of a climbing robot that uses the HMA material for attaching and detaching its body to the environment. The robot is equipped with servomotors and thermal control units to actively vary the temperature of the material, and the coordination of these components enables the robot to walk against the gravitational forces even with a relatively large body weight. A real-world platform is used to demonstrate locomotion on a vertical wall, and the experimental result shows the feasibility and overall performances of this approach. © 2013 Elsevier B.V. All rights reserved.

The Effects of Roughness on Adhesion Hysteresis

Adhesion hysteresis is defined as the difference between the work needed to separate two surfaces and that originally gained on bringing them together. Adhesion hysteresis is a common phenomenon in most surface/interface interactions. This paper studies the effects of surface roughness on adhesion hysteresis. We assumed that the surface asperity height distribution is Gaussian. Numerical simulations based on Fuller's model showed that adhesion hysteresis depended upon a single dimensionless parameter, the adhesion parameter, which represents the statistical average of a competition between the compressive forces exerted by the higher asperities, which are trying to separate the surfaces, and the adhesion forces of the lower asperities which are trying to hold the surfaces together. (C) Koninklijke Brill NV, Leiden, 2010

Measuring the adhesion force on natural fibre surface using scanning probe microscopy

This work has focused on measuring the adhesion forces on both untreated and atmospheric helium plasma treated single jute fibre surfaces using scanning probe microscopy (SPM). The measurements were conducted on three differently aged surfaces for one week, three weeks and six weeks using a standard silicon nitride tip in force-volume (f-v) mode. Up to 256 adhesion data points were collected from various locations on the surface of the studied fibres using in-house developed software and the resulting data were statistically analysed by the histogram method. Results obtained from this analysis method were found to be very consistent with a small statistical variation. The work of adhesion, Wa, was calculated from measured adhesion force using the Johnson–Kendall–Roberts (JKR) and Derjaguin–Muller–Toporov (DMT) models. Increases in both adhesion force and work of adhesion were observed on jute fibre with certain levels of atmospheric plasma treatment and ageing time.

Influence of Particle Size, Applied Compression, and Substratum Material on Particle-Surface Adhesion Force Using the Centrifuge Technique

The centrifuge technique was used to investigate the influence of particle size, applied compression, and substrate material (stainless steel, glass, Teflon, and poly(vinyl chloride)) on particle-surface adhesion force. For this purpose, phosphatic rock (rho(p) = 3090 kg/m(3)) and manioc starch particles (rho(p) = 1480 kg/m(3)) were used as test particles. A microcentrifuge that reached a maximum rotation speed of 14 000 rpm and which contained specially designed centrifuge tubes was used in the adhesion force measurements. The curves showed that the adhesion force profile followed a normal log distribution. The adhesion force increased linearly with particle size and with the increase of each increment of compression force. The manioc starch particles presented greater adhesion forces than the phosphatic rock particles for all particle sizes studied. The glass substrate showed a higher adherence than the other materials, probably due to its smoother topographic surface roughness in relation to the other substrata.