Mapping the mechanical properties of biomaterials on different length scales: depth-sensing indentation and AFM based nanoindentation

Rettler, Erik F.-J.; Hoeppener, Stephanie; Sigusch, Bernd W.; Schubert, Ulrich S.

doi:10.1039/c3tb20120a

Cited by 53 publications

(34 citation statements)

References 140 publications

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“…Review articles and handbooks provide a good starting point for basic principles of the method (35,38,39,(48)(49)(50)(51)(52)(53)(54)(55)(56)(57)(58)(59)(60)(61). However, it is the author's experience that there is a common set of misconceptions and errors in the application of nanoindentation in pharmaceutical technology.…”

Section: Nanoindentationmentioning

confidence: 99%

Application of instrumented nanoindentation in preformulation studies of pharmaceutical active ingredients and excipients

2016

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Application of instrumented nanoindentation in preformulation studies of pharmaceutical active ingredients and excipients # Nanoindentation allows quantitative determination of a material's response to stress such as elastic and plastic deformation or fracture tendency. Key instruments that have enabled great advances in nanomechanical studies are the instrumented nanoindenter and atomic force microscopy. The versatility of these instruments lies in their capability to measure local mechanical response, in very small volumes and depths, while monitoring time, displacement and force with high accuracy and precision. This review highlights the application of nanoindentation for mechanical characterization of pharmaceutical materials in the preformulation phase (primary investigation of crystalline active ingredients and excipients). With nanoindentation, mechanical response can be assessed with respect to crystal structure. The technique is valuable for mechanical screening of a material at an early development phase in order to predict and better control the processes in which a material is exposed to stress such as milling and compression.

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Section: Nanoindentationmentioning

confidence: 99%

Application of instrumented nanoindentation in preformulation studies of pharmaceutical active ingredients and excipients

2016

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“…Furthermore, a variety of deformation modes can be studied by changing experimental time scales, indenter tip geometry and loading conditions. Because very small forces are applied, the technique is well suited for soft biomaterials (Karimzadeh and Ayatollahi, 2014;Rettler et al, 2013), such as hydrogels (Ebenstein and Pruitt, 2004;Kaufman et al, 2008), which due to their pliable and highly hydrated nature, are a challenge to characterise using macro-scale techniques. Finally, given that pathological and ageing tissues are known to exhibit altered mechanical properties (Derby and Akhtar, 2015;DeWall et al, 2012), this method is also attractive in the biomedical context as a potential diagnostic tool or for intelligent scaffold design (Albert et al, 2013;Lyyra et al, 1995;Mattei et al, 2015).…”

Section: Introductionmentioning

confidence: 99%

The nano-epsilon dot method for strain rate viscoelastic characterisation of soft biomaterials by spherical nano-indentation

Mattei

Gruca

Rijnveld

et al. 2015

Journal of the Mechanical Behavior of Biomedical Materials

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Nano-indentation is widely used for probing the micromechanical properties of materials. Based on the indentation of surfaces using probes with a well-defined geometry, the elastic and viscoelastic constants of materials can be determined by relating indenter geometry and measured load and displacement to parameters which represent stress and deformation. Here we describe a method to derive the viscoelastic properties of soft hydrated materials at the micro-scale using constant strain rates and stress-free initial conditions. Using a new self-consistent definition of indentation stress and strain and corresponding unique depth-independent expression for indentation strain rate, the epsilon dot method, which is suitable for bulk compression testing, is transformed to nano-indentation. We demonstrate how two materials can be tested with a displacement controlled commercial nano-indentor using the nano-espilon dot method (nano-ε̇M) to give values of instantaneous and equilibrium elastic moduli and time constants with high precision. As samples are tested in stress-free initial conditions, the nano-ε̇M could be useful for characterising the micro-mechanical behaviour of soft materials such as hydrogels and biological tissues at cell length scales.

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“…By integrating AFM and nano-DMA, both morpho and nanomechanical properties can be obtained. In particular, biological sample systems resemble complex biochemical and biophysic architectures (Rettler et al, 2013).…”

Section: Introductionmentioning

confidence: 99%

Ions-modified nanoparticles affect functional remineralization and energy dissipation through the resin-dentin interface

Toledano

Osorio

et al. 2017

Journal of the Mechanical Behavior of Biomedical Materials

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The aim of this study was to evaluate changes in the mechanical and chemical behavior, and bonding ability at dentin interfaces infiltrated with polymeric nanoparticles (NPs) prior to resin application. Dentin surfaces were treated with 37% phosphoric acid followed by application of an ethanol suspension of NPs, Zn-NPs or Ca-NPs followed by the application of an adhesive, Single Bond (SB). Bonded interfaces were stored for 24 h, submitted to microtensile bond strength test, and evaluated by scanning electron microscopy. After 24 h and 21 d of storage, the whole resin-dentin interface adhesive was evaluated using a Nano-DMA. Complex modulus, storage modulus and tan delta (δ) were assessed. AFM imaging and Raman analysis were performed. Bond strength was not affected by NPs infiltration. After 21 d of storage, tan δ generally decreased at Zn-NPs/resin-dentin interface, and augmented when Ca-NPs or non-doped NPs were used. When both Zn-NPs and Ca-NPs were employed, the storage modulus and complex modulus decreased, though both moduli increased at the adhesive and at peritubular dentin after Zn-NPs infiltration. The phosphate and the carbonate peaks, and carbonate substitution, augmented more at interfaces promoted with Ca-NPs than with Zn-NPs after 21 d of storage, but crystallinity did not differ at created interfaces with both ions-doped NPs. Crosslinking of collagen and the secondary structure of collagen improved with Zn-NPs resin-dentin infiltration. Ca-NPs-resin dentin infiltration produced a favorable dissipation of energy with minimal stress concentration trough the crystalline remineralized resin-dentin interface, causing minor damage at this structure.

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Mapping the mechanical properties of biomaterials on different length scales: depth-sensing indentation and AFM based nanoindentation

Cited by 53 publications

References 140 publications

Application of instrumented nanoindentation in preformulation studies of pharmaceutical active ingredients and excipients

Application of instrumented nanoindentation in preformulation studies of pharmaceutical active ingredients and excipients

The nano-epsilon dot method for strain rate viscoelastic characterisation of soft biomaterials by spherical nano-indentation

Ions-modified nanoparticles affect functional remineralization and energy dissipation through the resin-dentin interface

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