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Measurement of the microstructural fracture toughness of cortical bone using indentation fracture

https://doi.org/10.1016/j.jbiomech.2007.04.020Get rights and content

Abstract

The purpose of this work is to investigate the use of indentation fracture as a method of measuring toughness at the microscale in cortical bone. Indentation fracture employs sharp indenters to initiate cracks, whose length can be used to calculate the toughness of the material. Only a cube corner indenter tip is found to initiate cracks at a suitable size scale for microstructural measurement. Cracks from 7 to 56 μm in length are produced using loads from 0.05 to 3 N. Preliminary data predicts rising toughness with increasing crack length (rising R-curve behaviour) at the microscale. This technique provides a new insight into fracture in cortical bone since it allows the investigator to observe mechanisms and measure toughness at a size scale at which in vivo damage is known to exist.

Introduction

Measurements of bone quantity, while useful in predicting fracture risk, cannot fully explain incidence of fracture (Hernandez and Keaveny, 2006). Other architectural factors such as geometry and material properties must therefore be influential. These factors are categorised as measures of bone quality (Hernandez and Keaveny, 2006). In order to improve our ability to assess fracture risk, our understanding of the contribution of bone quality must first be improved (Rho et al., 1998; Zioupos and Currey, 1998; Hernandez and Keaveny, 2006). One measure of quality that is directly related to the fracture of materials is fracture toughness.

Microcracks due to in vivo loading are known to exist in bone (Schaffler et al., 1989). In an effort to understand microcrack growth and fracture in bone, various methods have been used to measure fracture toughness, a review of which can be found in Yan et al. (2006). While these studies have measured the toughness of bone at a macroscale and revealed its variation with crack extension (rising R-curve behaviour), the techniques employed have not allowed a microstructural toughness measurement. It has recently been suggested that “in situ” measurement of toughness of the bone matrix at the microscale is the next stage in the examination of microcracks and bone quality (Zioupos, 2005).

Indentation fracture was first proposed by Palmqvist (1962) and developed by Evans et al. (1980) for the measurement of the microstructural toughness of ceramics. It has since been used to measure toughness of a wide range of materials and to investigate R-curve behaviour (Ramachandran and Shetty, 1991; Bleise and Steinbrech, 1994; Smith and Scattergood, 1996; Xu et al., 2000). Biological materials, such as enamel and dentin, often considered analogous to bone, because of their structure and anisotropy have also been the subject of studies using indentation fracture (Hassan et al., 1981; White et al., 2005). The technique employs a sharp indenter to grow cracks in a material at the microstructural level. The length of these cracks can then be used to calculate the toughness of the material using an empirical relation. Indentation fracture has some major advantages over traditional toughness testing methods: it allows measurement at the microscale. There is no need for machining microspecimens. The technique is extremely efficient, allowing many measurements on a small quantity of material. Finally, in the case of bone, the cracks produced are of the same size scale as those observed in vivo, and may therefore provide a more relevant insight into the nature of damage in bone.

The purpose of this study was to investigate indentation fracture as a method of measuring the microstructural toughness of cortical bone.

Section snippets

Specimen preparation

Longitudinal–transverse and transverse sections were excised from the middle diaphysis of four ovine tibiae using a Buhler Isomet low speed saw. The sections were then embedded in an epoxy resin with a low curing temperature (Buehler Epoxicure, 28 °C) and allowed to cure overnight at room temperature (Rho et al., 1999; Turner et al., 1999; Zysset et al., 1999; Fan et al., 2002). Following embedding, the samples were ground and polished to a surface roughness of 0.05 μm and ultrasonically cleaned

Results

Measured values of modulus and hardness (see Table 1) were in the same range as those reported previously in nanoindentation studies of human cortical bone (Rho et al., 1998; Rho and Pharr, 1999; Zysset et al., 1999; Fan et al., 2002). It was found that only the cube-corner indenter tip produced cracks. This is consistent with previous nanoindentation studies on bone in which no cracks have been reported using the Berkovich or Vickers tip. Pharr (1998) reports that the cube-corner tip can

Discussion

The goal of this study was to investigate indentation fracture as a means of measuring the microstructural fracture toughness of cortical bone. Using a cube-corner indenter, it was possible to produce cracks which could be used to calculate microscale toughness.

The measured toughness values of the samples were found to be lower than the range of values reported previously in literature which are typically 2.1–6.0 MPa√m (Yan et al., 2006). These studies, however, involved the growth of much

Conflict of interest

There is no conflict of interest.

Acknowledgement

The authors wish to acknowledge funding from the Programme for Research in Third Level Institutions (PRTLI), administered by the Higher Education Authority (HEA).

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    Scratch test has been routinely used in various industrial domains and engineering applications to characterize adhesion and fracture toughness of surface coatings and layers (e.g. organic coatings [108], automotive polymeric clearcoats [109], boride layers [110] and nickel boride layer [111]), scratch resistance, failure/removal and mechanical performance of bulk material (e.g. metals [5], glass [7] and ceramic tiles [112]). Scratch test has many advantages over conventional approaches: (1) fracture toughness can be conveniently obtained with good reproducibility and minimal uncertainty (e.g. absence of notch sensitivities), since the data required can be experimentally measured with high accuracy, avoiding the subjectivity of measurement of crack lengths in indentation technique [59,113,114]; (2) sample preparation is much simpler, since pre-crack or notch (measurement of fracture toughness is sensitive to machine characteristics [115], notch radius/sharpness, thickness of single edge notched specimen [97,116,117], loading condition, geometry and type of specimen [118–121]) that is normally required in compact tension and three-point bending tests is not required; (3) it is costless compared to other methods, which require many specimens and statistical analysis, since material supply is minimal, and distribution of fracture properties of sample surface can be quantified from multiple measurements on one specimen [87]. However, whether scratch-based approach can be applied in assessing fracture toughness of material is still under debate and in need of stress analysis, since hydrostatic stress ahead of the probe is expected to determine the mechanics of defect initiation [81,122], and stress magnitude at rear part of the indenter is even larger than that at front part of the indenter [9].

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