A new framework for characterization of poroelastic materials using indentation

To characterize a poroelastic material, typically an indenter is pressed onto the surface of the material with a ramp of a finite approach velocity followed by a hold where the indenter displacement is kept constant This leads to deformation of the porous matrix, pressurization of the interstitial fluid and relaxation due to redistribution of fluid through the pores. In most studies the poroelastic properties, including elastic modulus, Poisson ratio and poroelastic diffusion coefficient, are extracted by assuming an instantaneous step indentation. However, exerting step like indentation is not experimentally possible and usually a ramp indentation with a finite approach velocity is applied. Moreover, the poroelastic relaxation time highly depends on the approach velocity in addition to the poroelastic diffusion coefficient and the contact area. Here, we extensively studied the effect of indentation velocity using finite element simulations which has enabled the formulation of a new framework based on a master curve that incorporates the finite rise time. To verify our novel framework, the poroelastic properties of two types of hydrogels were extracted experimentally using indentation tests at both macro and micro scales. Our new framework that is based on consideration of finite approach velocity is experimentally easy to implement and provides more accurate estimation of poroelastic properties

MECHANICAL CHARACTERIZATION OF NORMAL AND CANCEROUS BREAST TISSUE SPECIMENS USING ATOMIC FORCE MICROSCOPY

Breast cancer is one of the most common malignancies among women worldwide. Conventional breast cancer diagnostic methods involve needle-core biopsy procedures, followed by careful histopathological inspection of the tissue specimen by a pathologist to identify the presence of cancerous lesions. However, such inspections are primarily qualitative and depend on the subjective impressions of observers. The goal of this research is to develop approaches for obtaining quantitative mechanical signatures that can accurately characterize malignancy in pathological breast tissue. The hypothesis of this research is that by using contact-mode Atomic Force Microscopy (AFM), it is possible to obtain differentiable measures of stiffness of normal and cancerous tissue specimens. This dissertation summarizes research carried out in addressing key experimental and computational challenges in performing mechanical characterization on breast tissue. Firstly, breast tissue specimens studied were 600 um in diameter, about six times larger than the range of travel of conventional AFM X-Y stages used for imaging applications. To scan tissue properties across large ranges, a semi automated image-guided positioning system was developed that can be used to perform AFM probe-tissue alignment across distances greater than 100 um at multiple magnifications. Initial tissue characterization results indicate that epithelial tissue in cancer specimens display increased deformability compared to epithelial tissue in normal specimens. Additionally, it was also observed that the tissue response depends on the patient from whom the specimens were acquired. Another key challenge addressed in this dissertation is accurate data analysis of raw AFM data for characterization purposes. Two sources of uncertainty typically influence data analysis of AFM force curves: the AFM probe's spring constant and the contact point of an AFM force curve. An error-in-variable based Bayesian Changepoint algorithm was developed to quantify estimation errors in the tissue's elastic properties due to these two error sources. Next, a parametric finite element modeling based approach was proposed in order to account for spatial heterogeneity in the tissue response. By using an exponential hyperelastic material model, it was shown that it is possible to obtain more accurate material properties of tissue specimens as opposed to existing analytical contact models. The experimental and computational strategies proposed in this dissertation could have a significant impact on high-throughput quantitative studies of biomaterials, which could elucidate various disease mechanisms that are phenotyped by their mechanical signatures

Nanoindentation testing of soft polymers : computation, experiments and parameters identification

Since nanoindentation technique is able to measure the mechanical properties of extremely thin layers and small volumes with high resolution, it also became one of the important testing techniques for thin polymer layers and coatings. This dissertation is focusing on the characterization of polymers using nanoindentation, which is dealt with numerical computation, experiments and parameters identification. An analysis procedure is developed with the FEM based inverse method to evaluate the hyperelasticity and time-dependent properties. This procedure is firstly verified with a parameters re-identification concept. An important issue in this dissertation is to take the error contributions in real nanoindentation experiments into account. Therefore, the effects of surface roughness, adhesion force, friction and the real shape of the tip are involved in the numerical model to minimize the systematic error between the experimental responses and the numerical predictions. The effects are quantified as functions or models with corresponding parameters to be identified. Finally, data from uniaxial or biaxial tensile tests and macroindentation tests are taken into account. The comparison of these different loading situations provides a validation of the proposed material model and a deep insight into nanoindentation of polymers.Da Nanoindentation die Messung der mechanischen Eigenschaften von dünnen Schichten und kleinen Volumen mit hoher Auflösung ermöglicht, hat sich diese Messmethode zu einer der wichtigsten Testmethoden für dünne Polymerschichten und -beschichtungen entwickelt. Diese Dissertation konzentriert sich auf die Charakterisierung von Polymeren mittels Nanoindentation, die in Form von numerischen Berechnungen, Experimenten und Parameteridentifikationen behandelt wird. Es wurde ein Auswertungsverfahren mit einer FEM basierten inversen Methode zur Berechnung der Hyperelastizität und der zeitabhängigen Eigenschaften entwickelt. Dieses Verfahren wird zunächst mit einem Konzept der Parameter Re-Identifikation verifiziert. Fehlerquellen wie Oberflächenrauheit, Adhäsionskräfte, Reibung und die tatsächlichen Form der Indenterspitze werden in das numerische Modell eingebunden, um die Abweichungen der numerischen Vorhersagen von den experimentellen Ergebnissen zu minimieren. Diese Einflüsse werden als Funktionen oder Modelle mit dazugehörigen, zu identifizierenden Parametern, quantifiziert. Abschließend werden Messwerte aus uni- oder biaxialen Zugversuchen und Makroindentationsversuchen betrachtet. Der Vergleich dieser verschiedenen Belastungszustände liefert eine Bestätigung des vorgeschlagenen Materialmodells und verschafft einen tieferen Einblick in die bei der Nanoindentation von Polymeren ablaufenden Mechanismen

Mechanics of Micro- and Nano-Size Materials and Structures

For this reprint, we intend to cover theoretical as well as experimental works performed on small scale to predict the material properties and characteristics of any advanced and metamaterials. New studies on mechanics of small-scale structures such as MEMS/NEMS, carbon and non-carbon nanotubes (e.g., CNTs, Carbon nitride, and Boron nitride nanotubes), micro/nano-sensors, nanocomposites, macrocomposites reinforced by micro-/nano-fillers (e.g., graphene platelets), etc., are included in this reprint

A Review on Mechanics and Mechanical Properties of 2D Materials - Graphene and Beyond

Since the first successful synthesis of graphene just over a decade ago, a variety of two-dimensional (2D) materials (e.g., transition metal-dichalcogenides, hexagonal boron-nitride, etc.) have been discovered. Among the many unique and attractive properties of 2D materials, mechanical properties play important roles in manufacturing, integration and performance for their potential applications. Mechanics is indispensable in the study of mechanical properties, both experimentally and theoretically. The coupling between the mechanical and other physical properties (thermal, electronic, optical) is also of great interest in exploring novel applications, where mechanics has to be combined with condensed matter physics to establish a scalable theoretical framework. Moreover, mechanical interactions between 2D materials and various substrate materials are essential for integrated device applications of 2D materials, for which the mechanics of interfaces (adhesion and friction) has to be developed for the 2D materials. Here we review recent theoretical and experimental works related to mechanics and mechanical properties of 2D materials. While graphene is the most studied 2D material to date, we expect continual growth of interest in the mechanics of other 2D materials beyond graphene

Nonlinear indentation of second-order hyperelastic materials

The classical problem of indentation on an elastic substrate has found new applications in the field of the Atomic Force Microscopy. However, linearly elastic indentation models are not sufficiently accurate to predict the force–displacement relationship at large indentation depths. For hyperelastic materials, such as soft polymers and biomaterials, a nonlinear indentation model is needed. In this paper, we use second-order elasticity theory to capture larger amplitude deformations and material nonlinearity. We provide a general solution for the contact problem for deformations that are second-order in indentation amplitude with arbitrary indenter profiles. Moreover, we derive analytical solutions by using either parabolic or quartic surfaces to mimic a spherical indenter. The analytical prediction for a quartic surface agrees well with finite element simulations using a spherical indenter for indentation depths on the order of the indenter radius. In particular, the relative error between the two approaches is less than 1% for an indentation depth equal to the indenter radius, an order of magnitude less than that observed with models which are either first-order in indentation amplitude or those which are second-order in indentation amplitude but with a parabolic indenter profile

Optimization of Indentation for the Material Characterization of Soft PVA-Cryogels

Over the past few years a variety of clinical procedures aiming at tissue repair and other relevant therapies have been under active investigation [12,32]. Success of procedures aimed at soft tissue repair depend on the combined response of biochemical and biomechanical properties of the organs neighbouring the tissue [53]. Using human or animal cadaveric tissue for this purpose is very challenging due to issues pertaining to biodegradability and infection or biohazard risk factors [135,205].As such, tissue mimicking materials (e.g. Polyvinyl Alcohol Cryo-gel (PVA-C)) have been investigated to satisfy the need for the said clinical applications. Advantages of using tissue-mimicking materials include (a) biocompatibility, (b) being not biodegradable and long term shape preservation and (c) having similar biomechanical properties of human tissue [76,126]. To assess biomechanical compatibility of tissue mimicking materials, various mechanical testing techniques have been proposed. Among them, indentation testing has shown great potential for this purpose and it has been used broadly for tissue biomechanical characterization [158]. This method has become more popular because it allows for cost effective, non-destructive, quick, and quantitative assessment of soft tissue biomechanics [64,193]. Soft tissue is idealized as non-linear [46], isotropic [72] and incompressible [198] material. Given its interesting properties and biocompatibility, PVA-C has attracted a great deal of attention as a biocompatible material suitable for clinical applications such as tissue repair, tissue engineering etc. As such, many studies have been conducted to understand this material’s mechanical properties and its suitability for fabricating artificial cornea replacement [54], heart valve [90], lung [164], breast [167], kidney [169], brain [195], stomach [160], bladder [18], prostate [36] and articular cartilage [20] This stems from that this material has similar characteristics to human soft tissue [44,46,129]. Similar to biological tissues, the internal structure of PVA-C leads to nonlinear behavior [66, 80]. This nonlinearity becomes predominant while it undergoes large deformation [205]. Several analytical, semi-analytical and computational models have been proposed to understand tissue mechanical behavior, including its linear and nonlinear behavior, under indentation testing[60]. These include the methods proposed by Boussinesq [27],Sneddon[176],Hayes[77], Cao [34]. This thesis aims at gaining in-depth insight into the mechanical behavior of PVA-C under indentation testing. To this end it presents development of an inverse Finite Element (FE) techniques solved using numerical optimization to characterize the mechanical properties of PVA-C specimens. used to understand the indentation response of PVA-C at different thickness and conditions. The investigation reported in this thesis includes numerical analysis where displacement influence factor was employed in conjunction with linear elastic model of finite thickness. In the analysis, effects of Poisson’s ratio, specimen aspect ratio and relative indentation depth were investigated and a novel mathematical term was introduced to Sneddon’s equation. Results indicate that the developed models have been successful to characterize PVA-C material while they can be used effectively in characterizing the mechanical behavior of biological tissue specimens obtained from medical intervention

The development of a soft tissue mimicking hydrogel: Mechanical characterisation and 3D printing

Accurate tissue phantoms are difficult to design due to the complex hyperelastic, viscoelastic and biphasic properties of real soft tissues. The aim of this work is to demonstrate the tissue mimicking ability of a composite hydrogel (CH), constituting of poly(vinyl alcohol) (PVA) and phytagel (PHY), as a soft tissue phantom over a range mechanical properties, for a variety of biomedical and tissue engineering applications. Its compressive stress-strain behaviour, relaxation response, tensile impact stresses and surgical needle-tissue interactions were mapped and characterised with respect to its constituent hydrogel formulation. The mechanical characterisation of biological tissues was also investigated and the results were used as the ground truth for mimicking. The best mimicking hydrogel compositions were determined by combining the most relevant mechanical properties for each desired application. This thesis demonstrates the use of the tissue mimicking composite hydrogel formulations as tissue phantoms for various surgical procedures, including convection enhanced drug delivery, and traumatic brain injury studies. To expand the applications of the CH, a preliminary biological evaluation of the hydrogel was performed using human dermal fibroblasts. Cell seeded on the collagen-coated composite hydrogel showed good attachment and viability. Finally, a novel fabrication method with the aim of creating samples that replicate the anisotropic properties of biological tissues was developed. A cryogenic 3D printing method utilising the liquid to solid phase change of the composite hydrogel ink was achieved by rapidly cooling the ink solution below its freezing point. The setup was able to successfully create complex 3D brain mimicking material. The method was validated by showing that the mechanical and microstructural properties of the 3D printed material was well matched to its cast-moulded equivalent. This greatly widens the applications of the CH as a mechanically accurate tool for in-vitro testing and also demonstrates promise for future mechanobiology and tissue engineering studies.Open Acces