Focused ion-beam (FIB) fabrication of micro-sized pillars for microcompression test

Pillars were fabricated by focused-ion beam (FIB) in a dual beam scanning electron microscope (SEM, FEI Quanta 3D). A multi-step milling procedure was adopted to prepare the pillars using Ga+ ion beam operated at 30 kV. The beam current was reduced from 5 nA for coarse milling down to 50 pA for fine milling, to minimize the surface damage induced by the Ga+ ion beam. The pillars were imaged at 52° tilt angle by SEM prior to the microcompression tests.

Mechanical Behavior of Nano-crystalline Metallic Thin Films and Multilayers Under Microcompression

Microcompression tests were performed to determine the mechanical behavior of nano-crystalline Cu/Fe and Fe/Cu multilayers, as well as monolithic Cu and Fe thin films. The results show that the micropillars of pure Cu thin film bulge out under large compressive strains without failure, while those of pure Fe thin film crack near the top at low compressive strains followed by shear failure. For Cu/Fe and Fe/Cu multilayers, the Cu layers accommodate the majority of plastic deformation, and the geometry constraints imposed by Fe layers exaggerates the bulging in the Cu layers. However, the existence of ductile Cu layers does not improve the overall ductility of Cu/Fe and Fe/Cu multilayers. Cracking in the Fe layers directly lead to the failure of the multilayer micropillars, although the Cu layers have very good ductility. The results imply that suppressing the cracking of brittle layers is more important than simply adding ductile layers for improving the overall ductility of metallic multilayers.

The stimulation of healing within a rat calvarial defect by mPCL–TCP/collagen scaffolds loaded with rhBMP-2

Bone morphogenetic proteins (BMPs) have been widely investigated for their clinical use in bone repair and it is known that a suitable carrier matrix to deliver them is essential for optimal bone regeneration within a specific defect site. Fused deposited modeling (FDM) allows for the fabrication of medical grade poly 3-caprolactone/tricalcium phosphate (mPCL–TCP) scaffolds with high reproducibility and tailor designed dimensions. Here we loaded FDM fabricated mPCL–TCP/collagen scaffolds with 5 mg recombinant human (rh)BMP-2 and evaluated bone healing within a rat calvarial critical-sized defect. Using a comprehensive approach, this study assessed the newly regenerated bone employing microcomputed tomography (mCT), histology/histomorphometry, and mechanical assessments. By 15 weeks, mPCL–TCP/collagen/rhBMP-2 defects exhibited complete healing of the calvarium whereas the non- BMP-2-loaded scaffolds showed significant less bone ingrowth, as confirmed by mCT. Histomorphometry revealed significantly increased bone healing amongst the rhBMP-2 groups compared to non-treated scaffolds at 4 and 15 weeks, although the % BV/TV did not indicate complete mineralisation of the entire defect site. Hence, our study confirms that it is important to combine microCt and histomorphometry to be able to study bone regeneration comprehensively in 3D. A significant up-regulation of the osteogenic proteins, type I collagen and osteocalcin, was evident at both time points in rhBMP-2 groups. Although mineral apposition rates at 15 weeks were statistically equivalent amongst treatment groups, microcompression and push-out strengths indicated superior bone quality at 15 weeks for defects treated with mPCL–TCP/collagen/rhBMP-2. Consistently over all modalities, the progression of healing was from empty defect < mPCL–TCP/collagen < mPCL–TCP/collagen/rhBMP-2, providing substantiating data to support the hypothesis that the release of rhBMP-2 from FDM-created mPCL–TCP/collagen scaffolds is a clinically relevant approach to repair and regenerate critically-sized craniofacial bone defects. Crown Copyright 2008 Published by Elsevier Ltd. All rights reserved.

Mechanical behaviour of metallic thin films and multilayers at the micron/submicron scale

Mechanical behaviours of CuFe thin films and multilayers at micron scales were investigated by microcompression and nanoindentation tests. Experimental and modelling results provide essential understanding on the extrinsic size effects in polycrystalline metallic multilayers, which is critical for optimising mechanical properties of thin films and multilayers.

Experimental studies and modelling of the deformation behaviour of multiple nanolayers

Microcompression tests were performed on monolithic Cu and Fe thin films and a Cu/Fe multilayer that had each individual layer of 200 nm thick, to understand the mechanical behaviour of multiple nanolayers. The micron-sized pillars were prepared by focused-ion beam (FIB) technique and compressed with a flat punch in a nanoindenter. The flow curves of the monolithic Cu and Fe thin films and Cu/Fe multilayer were extracted from the microcompression tests. The monolithic Cu thin film bulges in the top region of the pillar, while the Fe thin film cracks due to its columnar grain structure. For the Cu/Fe multilayer, the ductile Cu layers accommodate the majority of plastic deformation upon compression, while cracking in the Fe layers leads to the failure of the multilayer. Finite element models of microcompression tests were also developed to provide insights into the deformation behaviours of the multilayer and monolithic thin films. © 2012 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Strain gradients in Cu-Fe thin films and multilayers during micropillar compression

Plastic strain gradients can influence the work-hardening behaviour of metals due to the accumulation of geometrically necessary discolations at the micron/submicron scale. A finite element model based on the conventional theory of mechanism-based strain-gradient plasticity has been developed to simulate the micropillar compression of Cu–Fe thin films and multilayers. The modelling results show that the geometric constraints lead to inhomogeneous deformation in the Cu layers, which agrees well with the bulging of Cu layers observed experimentally. Plastic strain gradients develop inside the individual layers, leading to extra work-hardening due to the accumulation of geometrically necessary dislocations. In the multilayer specimens, the Cu layers deform more severely than the Fe layers, resulting in the development of tensile stresses in the Fe layers. It is proposed that these tensile stresses are responsible for the development of micro-cracks in the Fe layers.

A micro-compression study of shape-memory deformation in U-13 at.% Nb

Microcompression specimens, 10–15 µm in diameter by 20–30 µm in height, were produced from individual parent grains in a polycrystalline U–13 at.%Nb shape-memory alloy using the focused ion beam technique. The specimens were tested in a nanoindentation instrument with a flat diamond tip to investigate stress–strain behavior as a function of crystallographic orientation. The results are in qualitative agreement with a single-crystal accommodation strain (Bain strain) model of the shape-memory effect for this alloy.