In Situ Laboratory-Based Transmission X-Ray Microscopy and Tomography of Material Deformation at the Nanoscale

Patterson, Brian M.; Cordes, Nikolaus L.; Henderson, Kevin; Mertens, James C.E.; Clarke, Amy J.; Hornberger, Benjamin; Merkle, Arno; Etchin, Sergey; Tkachuk, Andrei; Leibowitz, Marty; Trapp, David; Qiu, Wei; Zhang, Bosheng; Bale, Hrishikesh; Lu, Xuekun; Hartwell, Rebecca; Withers, Philip J.; Bradley, Robert S.

doi:10.1007/s11340-016-0197-3

Cited by 47 publications

(34 citation statements)

References 59 publications

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“…The typical resolution is of the order of 1 to 10 µm per voxel for micro-CT. Therefore x-ray microtomography is sometimes referred to as x-ray microscopy [55,177].…”

Section: Tomography and Laminographymentioning

confidence: 99%

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Digital Volume Correlation: Review of Progress and Challenges

et al. 2018

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3D imaging has become popular for analyzing material microstructures. When time lapse series of 3D pictures are acquired during a single experiment, it is possible to measure displacement fields via digital volume correlation (DVC), thereby leading to 4D results. Such ForewordThe present paper aims at reviewing the major developments in Digital Volume Correlation (DVC) over the past ten years. It follows the first review on DVC that was published in 2008 by its pioneer [11]. In the latter, the interested reader will find all the general principles associated with what is now called local DVC. They will not be recalled hereafter. In such approaches the region of interest is subdivided into small subvolumes that are independently registered. In addition to its wider use with local approaches, DVC has been extended to global approaches in which the displacement field is defined in a dense way over the region of interest. Kinematic bases using finite element discretizations have been selected. To further add mechanical content, elastic regularization has been introduced. Last, integrated approaches use kinematic fields that are constructed from finite element simulations with chosen constitutive equations. The material parameters (and/or boundary conditions) then become the quantities of interest.These various implementations assume different degrees of integration of mechanical knowledge about the analyzed experiment. First and foremost, DVC can be considered as a stand-alone technique, which has seen its field of applications grow over the last ten years. In this case the measured displacement fields and post-processed strain fields are reported. With the introduction of finite element based DVC, the measured displacement field is continuous. It is also a standalone technique. However, given the fact that it shares common kinematic bases with numerical simulations, it can be easily combined with the latter. One route is to require local satisfaction of equilibrium via mechanical regularization. Another route is to fully merge DVC analyses and numerical simulations via integrated approaches. Different examples will illustrate how these various integration steps can be tailored and what are the current challenges associated with various approaches.

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“…The typical resolution is of the order of 1 to 10 µm per voxel for micro-CT. Therefore x-ray microtomography is sometimes referred to as x-ray microscopy [55,177].…”

Section: Tomography and Laminographymentioning

confidence: 99%

“…Very recently, nanotomography was used to image mechanical tests in lab tomographs or synchrotron facilities. In particular, ex-situ [161] and in-situ [177] indentation tests were analyzed.…”

Section: In-situ Testsmentioning

confidence: 99%

Digital Volume Correlation: Review of Progress and Challenges

et al. 2018

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“…This study looks at the interplay between crack initiation, microfracture and plastic deformation in relation to the local microstructure, namely the tubules and collagen fibers using in situ 3D X-ray nano-CT indentation. In order to examine the effect of tubule orientation samples are indented using a customised nano-mechanical test rig [54] in three different orientations (0°, 45°and 70°to the long axis of the tubules). Our aim is to develop a better understanding of the crack-tip behaviour in relation to the dentin microstructure during the early stages of crack growth.…”

Section: Introductionmentioning

confidence: 99%

Anisotropic Crack Propagation and Deformation in Dentin Observed by Four-Dimensional X-ray Nano-Computed Tomography

Fernández

Bradley

et al. 2019

SSRN Journal

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a b s t r a c tUnderstanding the cracking behaviour of biological composite materials is of practical importance. This paper presents the first study to track the interplay between crack initiation, microfracture and plastic deformation in three dimensions (3D) as a function of tubule and collagen fibril arrangement in elephant dentin using in situ X-ray nano-computed tomography (nano-CT). A nano-indenter with a conical tip has been used to incrementally indent three test-pieces oriented at 0°, 45°and 70°to the long axis of the tubules (i.e. radial to the tusk). For the 0°sample two significant cracks formed, one of which linked up with microcracks in the axial-radial plane of the tusk originating from the tubules and the other one occurred as a consequence of shear deformation at the tubules. The 70°test-piece was able to bear the greatest loads despite many small cracks forming around the indenter. These were diverted by the microstructure and did not propagate significantly. The 45°test-piece showed intermediate behaviour.In all cases strains obtained by digital volume correlation were well in excess of the yield strain (0.9%), indeed some plastic deformation could even be seen through bending of the tubules. The hoop strains around the conical indenter were anisotropic with the smallest strains correlating with the primary collagen orientation (axial to the tusk) and the largest strains aligned with the hoop direction of the tusk. Statement of SignificanceThis paper presents the first comprehensive study of the anisotropic nature of microfracture, crack propagation and deformation in elephant dentin using time-lapse X-ray nano-computed tomography. To unravel the interplay of collagen fibrils and local deformation, digital volume correlation (DVC) has been applied to map the local strain field while the crack initiation and propagation is tracked in real time. Our results highlight the intrinsic and extrinsic shielding mechanisms and correlate the crack growth behavior in nature to the service requirement of dentin to resist catastrophic fracture. This is of wide interest not just in terms of understanding dentin fracture but also can extend beyond dentin to other anisotropic structural composite biomaterials such as bone, antler and chitin.

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“…X-ray microtomography has been applied both at synchrotron sources (Babout et al, 2006;Connolly et al, 2006) and using laboratory systems (Burnett et al, 2015) to study corrosion processes over time at the micrometre scale. Recently, it has become possible to undertake time-lapse imaging of regions of interest around 50 µm in dimension at resolutions of ß50 nm or better using laboratory nano-CT systems (Patterson et al, 2016). However, to date very little work (Krebs et al, 2015) has exploited laboratory-based x-ray nano-CT for studying the corrosion and protection of metallic materials.…”

Section: Introductionmentioning

confidence: 99%

Time‐lapse lab‐based x‐ray nano‐CT study of corrosion damage

Bradley

Liu

Burnett

et al. 2017

Journal of Microscopy

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General rightsCopyright and moral rights for the publications made accessible in the Research Explorer are retained by the authors and/or other copyright owners and it is a condition of accessing publications that users recognise and abide by the legal requirements associated with these rights. Takedown policy ABSTRACTAn experimental protocol (workflow) has been developed for time-lapse x-ray nanotomography (nano-CT) imaging of environmentally-driven morphological changes to materials. Two case studies are presented. Firstly, the leaching of nanoparticle corrosion inhibitor pigment from a polymer coating was followed over 14 days, while in the second case the corrosion damage to an AA2099 aluminium alloy was imaged over 12 hours. The protocol includes several novel aspects relevant to nano-CT with the use of a combination of x-ray absorption and phase contrast data to provide enhanced morphological and composition information, and hence reveal the best information to provide new insights into the changes of different phases over time.For the pigmented polymer coating containing nominally strontium aluminium polyphosphate, the strontium-rich components within the materials are observed to leach extensively while the aluminium-rich components are more resistant to dissolution. In the case of AA2099 it is found that the initial grain boundary corrosion is driven by the presence of copper-rich phases and is then followed by the corrosion of grains of specific orientation.

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In Situ Laboratory-Based Transmission X-Ray Microscopy and Tomography of Material Deformation at the Nanoscale

Cited by 47 publications

References 59 publications

Digital Volume Correlation: Review of Progress and Challenges

Digital Volume Correlation: Review of Progress and Challenges

Anisotropic Crack Propagation and Deformation in Dentin Observed by Four-Dimensional X-ray Nano-Computed Tomography

Time‐lapse lab‐based x‐ray nano‐CT study of corrosion damage

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