Imperial College London

ProfessorPeterLee

Faculty of EngineeringDepartment of Materials

Visiting Professor
 
 
 
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Contact

 

+44 (0)20 7594 6801p.d.lee

 
 
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Location

 

102Royal School of MinesSouth Kensington Campus

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Summary

 

Publications

Publication Type
Year
to

521 results found

Ma L, Slater T, Dowey PJ, Yue S, Rutter EH, Taylor KG, Lee PDet al., 2018, Hierarchical integration of porosity in shales, Scientific Reports, Vol: 8, ISSN: 2045-2322

Pore characterization in shales is challenging owing to the wide range of pore sizes and types present. Haynesville-Bossier shale (USA) was sampled as a typical clay-bearing siliceous, organic-rich, gas-mature shale and characterized over pore diameters ranging 2 nm to 3000 nm. Three advanced imaging techniques were utilized correlatively, including the application of Xe+ plasma focused ion beam scanning electron microscopy (plasma FIB or PFIB), complemented by the Ga+ FIB method which is now frequently used to characterise porosity and organic/inorganic phases, together with transmission electron microscope tomography of the nano-scale pores (voxel size 0.6 nm; resolution 1–2 nm). The three pore-size scales each contribute differently to the pore network. Those <10 nm (greatest number), 10 nm to 100 nm (best-connected hence controls transport properties), and >100 nm (greatest total volume hence determines fluid storativity). Four distinct pore types were found: intra-organic, organic-mineral interface, inter-mineral and intra-mineral pores were recognized, with characteristic geometries. The whole pore network comprises a globally-connected system between phyllosilicate mineral grains (diameter: 6–50 nm), and locally-clustered connected pores within porous organic matter (diameter: 200–800 nm). Integrated predictions of pore geometry, connectivity, and roles in controlling petrophysical properties were verified through experimental permeability measurements.

Journal article

Wang Y, Liu B, Yan K, Wang M, Kabra S, Chiu Y-L, Dye D, Lee PD, Liu Y, Cai Bet al., 2018, Probing deformation mechanisms of a FeCoCrNi high-entropy alloy at 293 and 77 K using in situ neutron diffraction, Acta Materialia, Vol: 154, Pages: 79-89, ISSN: 1359-6454

The deformation responses at 77 and 293 K of a FeCoNiCr high-entropy alloy, produced by a powder metallurgy route, are investigated using in situ neutron diffraction and correlative transmission electron microscopy. The strength and ductility of the alloy are significant improved at cryogenic temperatures. The true ultimate tensile strength and total elongation increased from 980 MPa to 45% at 293 K to 1725 MPa and 55% at 77 K, respectively. The evolutions of lattice strain, stacking fault probability, and dislocation density were determined via quantifying the in situ neutron diffraction measurements. The results demonstrate that the alloy has a much higher tendency to form stacking faults and mechanical twins as the deformation temperature drops, which is due to the decrease of stacking fault energy (estimated to be 32.5 mJ/m2 and 13 mJ/m2 at 293 and 77 K, respectively). The increased volume faction of nano-twins and twin-twin intersections, formed during cryogenic temperature deformation, has been confirmed by transmission electron microscopy analysis. The enhanced strength and ductility at cryogenic temperatures can be attributed to the increased density of dislocations and nano-twins. The findings provide a fundamental understanding of underlying governing mechanistic mechanisms for the twinning induced plasticity in high entropy alloys, paving the way for the development of new alloys with superb resistance to cryogenic environments.

Journal article

Wang H, Cai B, Pankhurst MJ, Zhou T, Kashyap Y, Atwood R, Le Gall N, Lee P, Drakopoulos M, Sawhney Ket al., 2018, X-ray phase-contrast imaging with engineered porous materials over 50keV, Journal of Synchrotron Radiation, Vol: 25, Pages: 1182-1188, ISSN: 0909-0495

X-ray phase-contrast imaging can substantially enhance image contrast for weakly absorbing samples. The fabrication of dedicated optics remains a major barrier, especially in high-energy regions (i.e. over 50 keV). Here, the authors perform X-ray phase-contrast imaging by using engineered porous materials as random absorption masks, which provides an alternative solution to extend X-ray phase-contrast imaging into previously challenging higher energy regions. The authors have measured various samples to demonstrate the feasibility of the proposed engineering materials. This technique could potentially be useful for studying samples across a wide range of applications and disciplines.

Journal article

Guo E, Shuai S, Kazantsev D, Karagadde S, Phillion AB, Jing T, Li W, Lee PDet al., 2018, The influence of nanoparticles on dendritic grain growth in Mg alloys, ACTA MATERIALIA, Vol: 152, Pages: 127-137, ISSN: 1359-6454

Melt processing offers a cost effective method for producing metal matrix nanocomposite (MMNC) components; however, the influence of nanoparticles on the evolving microstructure during solidification is still not well understood. In this study, the effect of SiC nanoparticles on α-Mg dendrite evolution in a Mg-25Zn-7Al (wt.%) alloy was investigated through 4D (three dimensions plus time) synchrotron tomographic quantification of solidification experiments conducted at different cooling rates with and without nanoparticles. Key features of the solidifying primary α-Mg dendritic grains were quantified, including grain morphology, size distribution, and dendrite tip velocity. To obtain the high-contrast tomography dataset necessary for structure quantification, a new image reconstruction and processing methodology was implemented. The results reveal that the addition of nanoparticles increases grain nucleation whilst restricting dendritic growth and altering the dendritic grain growth morphology. Using LGK model calculations, it is shown that these changes in solidification microstructure occur as a result of nanoparticle-induced restriction in Zn's effective diffusivity ahead of the dendrite tips, reducing tip velocity. The results both suggest the key phenomena required to be simulated when numerically modelling solidifying Mg-based MMNC and provide the data required to validate those models.

Journal article

Javaheri B, Razi H, Piles M, de Souza R, Chang Y-M, Maric-Mur I, Hopkinson M, Lee PD, Pitsillides AAet al., 2018, Sexually dimorphic tibia shape is linked to natural osteoarthritis in STR/Ort mice, Osteoarthritis and Cartilage, Vol: 26, Pages: 807-817, ISSN: 1063-4584

OBJECTIVES: Human osteoarthritis (OA) is detected only at late stages. Male STR/Ort mice develop knee OA spontaneously with known longitudinal trajectory, offering scope to identify OA predisposing factors. We exploit the lack of overt OA in female STR/Ort and in both sexes of parental, control CBA mice to explore whether early divergence in tibial bone mass or shape are linked to emergent OA. METHOD: We undertook detailed micro-CT comparisons of trabecular and cortical bone, multiple structural/architectural parameters and finite element modelling (FEM) of the tibia from male and female STR/Ort and CBA mice at 8-10 (pre-OA), 18-20 (OA onset) and 40 + weeks (advanced OA) of age. RESULTS: We found higher trabecular bone mass in female STR/Ort than in either OA-prone male STR/Ort or non-prone CBA mice. Cortical bone, as expected, showed greater cross-sectional area in male than female CBA, which surprisingly was reversed in STR/Ort mice. STR/Ort also exhibited higher cortical bone mass than CBA mice. Our analyses revealed similar tibial ellipticity, yet greater predicted resistance to torsion in male than female CBA mice. In contrast, male STR/Ort exhibited greater ellipticity than both female STR/Ort and CBA mice at specific cortical sites. Longitudinal analysis revealed greater tibia curvature and shape deviations in male STR/Ort mice that coincided with onset and were more pronounced in late OA. CONCLUSION: Generalised higher bone mass in STR/Ort mice is more marked in non OA-prone females, but pre-OA divergence in bone shape is restricted to male STR/Ort mice in which OA develops spontaneously.

Journal article

Bjerre MK, Azeem M, Lee PD, Hattel JH, Tiedje NSet al., 2018, Revisiting models for spheroidal graphite growth, Science and Processing of Cast Iron XI, Publisher: Trans Tech Publications, Pages: 118-124, ISSN: 0255-5476

Recent experiments resolved nucleation and growth of graphite during solidification of ductile cast iron in 3D and time using synchrotron X-ray tomography [1]. We use the experimental observations to analyse the relation between graphite growth rate and the state of the particle neighbourhood to pinpoint possible links between growth rate of individual graphite spheres and the overall solidification state. With this insight we revisit existing models for growth of spheroidal graphite and discuss possible modifications in order to describe the critical final stage of solidification correctly.

Conference paper

Polacci M, Arzilli F, La Spina G, Le Gall N, Cai B, Hartley ME, Di Genova D, Vo NT, Nonni S, Atwood RC, Llewellin EW, Lee PD, Burton MRet al., 2018, Crystallisation in basaltic magmas revealed via in situ 4D synchrotron X-ray microtomography, Scientific Reports, Vol: 8, Pages: 8377-8377, ISSN: 2045-2322

Magma crystallisation is a fundamental process driving eruptions and controlling the style of volcanic activity. Crystal nucleation delay, heterogeneous and homogeneous nucleation and crystal growth are all time-dependent processes, however, there is a paucity of real-time experimental data on crystal nucleation and growth kinetics, particularly at the beginning of crystallisation when conditions are far from equilibrium. Here, we reveal the first in situ 3D time-dependent observations of crystal nucleation and growth kinetics in a natural magma, reproducing the crystallisation occurring in real-time during a lava flow, by combining a bespoke high-temperature environmental cell with fast synchrotron X-ray microtomography. We find that both crystal nucleation and growth occur in pulses, with the first crystallisation wave producing a relatively low volume fraction of crystals and hence negligible influence on magma viscosity. This result explains why some lava flows cover kilometres in a few hours from eruption inception, highlighting the hazard posed by fast-moving lava flows. We use our observations to quantify disequilibrium crystallisation in basaltic magmas using an empirical model. Our results demonstrate the potential of in situ 3D time-dependent experiments and have fundamental implications for the rheological evolution of basaltic lava flows, aiding flow modelling, eruption forecasting and hazard management.

Journal article

Javaheri B, Carriero A, Wood M, De Souza R, Lee PD, Shefelbine S, Pitsillides AAet al., 2018, Transient peak-strain matching partially recovers the age-impaired mechanoadaptive cortical bone response, SCIENTIFIC REPORTS, Vol: 8, ISSN: 2045-2322

Mechanoadaptation maintains bone mass and architecture; its failure underlies age-related decline in bone strength. It is unclear whether this is due to failure of osteocytes to sense strain, osteoblasts to form bone or insufficient mechanical stimulus. Mechanoadaptation can be restored to aged bone by surgical neurectomy, suggesting that changes in loading history can rescue mechanoadaptation. We use non-biased, whole-bone tibial analyses, along with characterisation of surface strains and ensuing mechanoadaptive responses in mice at a range of ages, to explore whether sufficient load magnitude can activate mechanoadaptation in aged bone. We find that younger mice adapt when imposed strains are lower than in mature and aged bone. Intriguingly, imposition of short-term, high magnitude loading effectively primes cortical but not trabecular bone of aged mice to respond. This response was regionally-matched to highest strains measured by digital image correlation and to osteocytic mechanoactivation. These data indicate that aged bone’s loading response can be partially recovered, non-invasively by transient, focal high strain regions. Our results indicate that old murine bone does respond to load when the loading is of sufficient magnitude, and bones’ age-related adaptation failure may be due to insufficient mechanical stimulus to trigger mechanoadaptation.

Journal article

Pankhurst MJ, Fowler R, Courtois L, Nonni S, Zuddas F, Atwood RC, Davis GR, Lee PDet al., 2018, Enabling three-dimensional densitometric measurements using laboratory source X-ray micro-computed tomography, SoftwareX, Vol: 7, Pages: 115-121, ISSN: 2352-7110

We present new software allowing significantly improved quantitative mapping of the three-dimensional density distribution of objects using laboratory source polychromatic X-rays via a beam characterisation approach (c.f. filtering or comparison to phantoms). One key advantage is that a precise representation of the specimen material is not required. The method exploits well-established, widely available, non-destructive and increasingly accessible laboratory-source X-ray tomography. Beam characterisation is performed in two stages: (1) projection data are collected through a range of known materials utilising a novel hardware design integrated into the rotation stage; and (2) a Python code optimises a spectral response model of the system. We provide hardware designs for use with a rotation stage able to be tilted, yet the concept is easily adaptable to virtually any laboratory system and sample, and implicitly corrects the image artefact known as beam hardening.

Journal article

Kazantsev D, Jorgensen JS, Andersen MS, Lionheart WRB, Lee PD, Withers PJet al., 2018, Joint image reconstruction method with correlative multi-channel prior for x-ray spectral computed tomography, INVERSE PROBLEMS, Vol: 34, ISSN: 0266-5611

Rapid developments in photon-counting and energy-discriminating detectors have the potential to provide an additional spectral dimension to conventional x-ray grayscale imaging. Reconstructed spectroscopic tomographic data can be used to distinguish individual materials by characteristic absorption peaks. The acquired energy-binned data, however, suffer from low signal-to-noise ratio, acquisition artifacts, and frequently angular undersampled conditions. New regularized iterative reconstruction methods have the potential to produce higher quality images and since energy channels are mutually correlated it can be advantageous to exploit this additional knowledge. In this paper, we propose a novel method which jointly reconstructs all energy channels while imposing a strong structural correlation. The core of the proposed algorithm is to employ a variational framework of parallel level sets to encourage joint smoothing directions. In particular, the method selects reference channels from which to propagate structure in an adaptive and stochastic way while preferring channels with a high data signal-to-noise ratio. The method is compared with current state-of-the-art multi-channel reconstruction techniques including channel-wise total variation and correlative total nuclear variation regularization. Realistic simulation experiments demonstrate the performance improvements achievable by using correlative regularization methods.

Journal article

Leung CLA, Marussi S, Atwood RC, Towrie M, Withers PJ, Lee PDet al., 2018, In situ X-ray imaging of defect and molten pool dynamics in laser additive manufacturing, Nature Communications, Vol: 9, ISSN: 2041-1723

The laser–matter interaction and solidification phenomena associated with laser additive manufacturing (LAM) remain unclear, slowing its process development and optimisation. Here, through in situ and operando high-speed synchrotron X-ray imaging, we reveal the underlying physical phenomena during the deposition of the first and second layer melt tracks. We show that the laser-induced gas/vapour jet promotes the formation of melt tracks and denuded zones via spattering (at a velocity of 1 m s−1). We also uncover mechanisms of pore migration by Marangoni-driven flow (recirculating at a velocity of 0.4 m s−1), pore dissolution and dispersion by laser re-melting. We develop a mechanism map for predicting the evolution of melt features, changes in melt track morphology from a continuous hemi-cylindrical track to disconnected beads with decreasing linear energy density and improved molten pool wetting with increasing laser power. Our results clarify aspects of the physics behind LAM, which are critical for its development.

Journal article

Fauchille AL, van den Eijnden AP, Ma L, Chandler M, Taylor KG, Madi K, Lee PD, Rutter Eet al., 2018, Variability in spatial distribution of mineral phases in the Lower Bowland Shale, UK, from the mm- to μm-scale: quantitative characterization and modelling, Marine and Petroleum Geology, Vol: 92, Pages: 109-127, ISSN: 1873-4073

The microstructure of a highly laminated Lower Bowland Shale sample is characterized at the micron-to millimeter scale, to investigate how such characterization can be utilized for microstructure-based modelling of the shale's geomechanical behavior. A mosaic of scanning electron microscope (SEM) back-scattered electron (BSE) images was studied. Mineral and organic content and their anisotropy vary between laminae, with a high variability in fracturing and multi-micrometer aggregates of feldspars, carbonates, quartz and organics. The different microstructural interface types and heterogeneities were located and quantified, demonstrating the microstructural complexity of the Bowland Shale, and defining possible pathways for fracture propagation. A combination of counting-box, dispersion, covariance and 2D mapping approaches were used to determine that the total surface of each lamina is 3 to 11 times larger than the scale of heterogeneities relative to mineral proportion and size. The dispersion approach seems to be the preferential technique for determining the representative elementary area (REA) of phase area fraction for these highly heterogeneous large samples, supported by 2D quantitative mapping of the same parameter. Representative microstructural models were developed using Voronoï tessellation using these characteristic scales. These models encapsulate the microstructural features required to simulate fluid flow through these porous Bowland Shales at the mesoscale.

Journal article

Wang YQ, Clark SJ, Janik V, Heenan RK, Venero DA, Yan K, McCartney DG, Sridhar S, Lee PDet al., 2018, Investigating nano-precipitation in a V-containing HSLA steel using small angle neutron scattering, Acta Materialia, Vol: 145, Pages: 84-96, ISSN: 1359-6454

Interphase precipitation (IPP) of nanoscale carbides in a vanadium-containing high-strength low-alloy steel has been investigated. Small angle neutron scattering (SANS) and transmission electron microscopy (TEM) were employed to characterize the precipitates and their size distributions in Fe-0.047C-0.2V-1.6Mn (in wt.%) alloy samples which had been austenitized, isothermally transformed at 700 °C for between 3 and 600 min and water quenched. TEM confirms that, following heat treatment, rows of vanadium-containing nanoscale interphase precipitates were present. Model-independent analysis of the nuclear SANS signal and model fitting calculations, using oblate spheroid and disc-shapes, were performed. The major axis diameter increased from 18 nm after 3 min to 35 nm after 600 min. Precipitate volume percent increased from 0.09 to 0.22 vol% over the same period and number density fell from 2 × 1021 to 5 × 1020 m−3. A limited number of measurements of precipitate maximum diameters from TEM images showed the mean value increased from 8 nm after 5 min to 28 nm after 600 min which is in reasonable agreement with the SANS data.

Journal article

Staines KA, Madi K, Javaheri B, Lee PD, Pitsillides AAet al., 2018, A Computed Microtomography Method for Understanding Epiphyseal Growth Plate Fusion, FRONTIERS IN MATERIALS, Vol: 4, ISSN: 2296-8016

The epiphyseal growth plate is a developmental region responsible for linear bone growth, in which chondrocytes undertake a tightly regulated series of biological pro-cesses. Concomitant with the cessation of growth and sexual maturation, the human growth plate undergoes progressive narrowing, and ultimately disappears. Despite the crucial role of this growth plate fusion “bridging” event, the precise mechanisms by which it is governed are complex and yet to be established. Progress is hindered by the current methods for growth plate visualization; these are invasive and largely rely on histological procedures. Here, we describe our non-invasive method utilizing synchro-tron X-ray computed microtomography for the examination of growth plate bridging, which ultimately leads to its closure coincident with termination of further longitudinal bone growth. We then apply this method to a dataset obtained from a benchtop micro computed tomography scanner to highlight its potential for wide usage. Furthermore, we conduct finite element modeling at the micron-scale to reveal the effects of growth plate bridging on local tissue mechanics. Employment of these 3D analyses of growth plate bone bridging is likely to advance our understanding of the physiological mechanisms that control growth plate fusion.

Journal article

Tiedje NS, Bjerre MK, Andriollo T, Azeem M, Zhang Y, Fæster S, Lee PD, Hattel JHet al., 2018, Use of high intensity X-ray analysis as tool to create new, fundamental models for phase transformations and residual stress in ductile cast iron, Pages: 239-240

Conference paper

Chuaypradit S, Puncreobutr C, Phillion AB, Fife JL, Lee PDet al., 2018, Quantifying the Effects of Grain Refiner Addition on the Solidification of Fe-Rich Intermetallics in Al-Si-Cu Alloys Using In Situ Synchrotron X-Ray Tomography, Light Metals Symposium at the 147th Annual TMS Meeting and Exhibition, Publisher: SPRINGER INTERNATIONAL PUBLISHING AG, Pages: 1067-1073, ISSN: 2367-1181

Conference paper

Maksimcuka J, Obata A, Sampson WW, Blanc R, Gao C, Withers PJ, Tsigkou O, Kasuga T, Lee PD, Poologasundarampillai Get al., 2017, X-ray Tomographic imaging of Tensile Deformation Modes of electrospun Biodegradable Polyester Fibers, Frontiers in Materials, Vol: 4, ISSN: 2296-8016

Electrospinning allows the production of fibrous networks for tissue engineering, drug delivery, and wound healing in health care. It enables the production of constructs with large surface area and a fibrous morphology that closely resembles the extracellular matrix of many tissues. A fibrous structure not only promotes cell attachment and tissue formation but could also lead to very interesting mechanical properties. Poly(3-hydroxybutyrate-co-4-hydroxybutyrate) (P(3HB-co-4HB)) is a biodegradable polyester that exhibits a large (>400%) elongation before failure. In this study, synchrotron X-ray phase contrast imaging was performed during tensile deformation to failure on a non-woven fiber mat of P(3HB-co-4HB) fibers. Significant reorientation of the fibers in the straining direction was observed, followed by localized necking and eventual failure. From an original average fiber diameter of 4.3 µm, a bimodal distribution of fiber diameter (modal diameters of 1.9 and 3.7 µm) formed after tensile deformation. Extensive localized necking (thinning) of fibers between (thicker) fiber–fiber contacts was found to be the cause for non-uniform thinning of the fibers, a phenomenon that is expected but has not been observed in 3D previously. The data presented here have implications not only in tissue regeneration but for fibrous materials in general.

Journal article

Ennis BL, Bos C, Aarnts MP, Lee PD, Jimenez-Melero Eet al., 2017, Work hardening behaviour in banded dual phase steel structures with improved formability, Materials Science and Engineering: A, Vol: 713, Pages: 278-286, ISSN: 0921-5093

In this work, we show how the presence of microstructural banding and segregation affects the work-hardening behaviour of a dual phase steel with improved formability. This steel contains chemical segregation inherited from the casting process. Our previously developed 3D cellular automaton model allowed us to design thermo-mechanical processes to either promote or suppress banding. The bands are properly described as in-plane sheets of martensite grains. Mechanical testing data revealed a significant reduction in tensile strength in banded structures for a similar level of ductility. The work-hardening behaviour in the pre-yield regime, including the yield strength itself, is not correlated to the incidence of segregation and/or microstructural banding. The reduction in ultimate tensile strength in banded structures stems from a reduced work-hardening capacity in the post-yield regime. This is due to increased austenite stability in the banded steels, coupled to the anisotropic strain localisation in the ferritic matrix between martensite bands.

Journal article

Xu W, Horsfield AP, Wearing D, Lee Pet al., 2017, Classical and quantum calculations of the temperature dependence of the free energy of argon, Computational Materials Science, Vol: 144, Pages: 36-41, ISSN: 0927-0256

The free energy is central to statistical mechanics and thermodynamics, and its accurate calculation via. computational modelling is important for a large number of applications, especially when its experimental value is hard to obtain. Several established and general methods for calculating the Helmholtz free energy across different length scales, including continuum, atomistic and quantum mechanical, are compared and analyzed. A computational approach is then proposed to calculate the temperature dependences of internal energy and absolute Helmholtz free energy for solid and liquid phases with the coupling of thermodynamic integration (TI) and harmonic approximation calculations from both classical molecular dynamics (MD) and density functional theory (DFT). We use the Lennard-Jones system as an example (i.e. argon) for the demonstration of the approach. It is observed that the free energy transits smoothly from being describable by the harmonic approximation to including anharmonic effects at a transition temperature around 0.56 Tm; below this temperature, the quantum behavior of atoms is important. At higher temperatures (T > 0.56 Tm), the TI and harmonic approximation results for the Helmholtz free energy functions become increasingly divergent with the increase of temperature. This work demonstrates that a multiscale approach employing TI, MD, and DFT can provide accurate calculations of the temperature dependence of absolute Helmholtz free energy for both solid and liquid phases.

Journal article

Disney CM, Madi K, Bodey AJ, Lee PD, Hoyland JA, Sherratt MJet al., 2017, Visualising the 3D microstructure of stained and native intervertebral discs using X-ray microtomography, Scientific Reports, Vol: 7, ISSN: 2045-2322

Intervertebral disc degeneration (IVDD) is linked to low back pain. Microstructural changes during degeneration have previously been imaged using 2D sectioning techniques and 3D methods which are limited to small specimens and prone to inducing artefacts from sample preparation. This study explores micro computed X-ray tomography (microCT) methods with the aim of resolving IVD 3D microstructure whilst minimising sample preparation artefacts. Low X-ray absorption contrast in non-mineralised tissue can be enhanced using staining and phase contrast techniques. A step-wise approach, including comparing three stains, was used to develop microCT for bovine tail IVD using laboratory and synchrotron sources. Staining successfully contrasted collagenous structures; however not all regions were stained and the procedure induced macroscopic structural changes. Phase contrast microCT of chemically fixed yet unstained samples resolved the nucleus pulposus, annulus fibrosus and constituent lamellae, and finer structures including collagen bundles and cross-bridges. Using the same imaging methods native tissue scans were of slightly lower contrast but free from sample processing artefacts. In the future these methods may be used to characterise structural remodelling in soft (non-calcified) tissues and to conduct in situ studies of native loaded tissues and constructs to characterise their 3D mechanical properties.

Journal article

Mosey H, Nunez JA, Goring A, Clarkin CE, Staines KA, Lee PD, Pitsillides AA, Javaheri Bet al., 2017, Sost Deficiency does not alter Bone's lacunar or Vascular Porosity in Mice, Frontiers in Materials, Vol: 4, ISSN: 2296-8016

SCLEROSTIN (Sost) is expressed predominantly in osteocytes acting as a negative regulator of bone formation. In humans, mutations in the SOST gene lead to skeletal overgrowth and increased bone mineral density, suggesting that SCLEROSTIN is a key regulator of bone mass. The function of SCLEROSTIN as an inhibitor of bone formation is further supported by Sost knockout (KO) mice which display a high bone mass with elevated bone formation. Previous studies have indicated that Sost exerts its effect on bone formation through Wnt-mediated regulation of osteoblast differentiation, proliferation, and activity. Recent in vitro studies have also suggested that SCLEROSTIN regulates angiogenesis and osteoblast-to-osteocyte transition. Despite this wealth of knowledge of the mechanisms responsible for SCLEROSTIN action, no previous studies have examined whether SCLEROSTIN regulates osteocyte and vascular configuration in cortices of mouse tibia. Herein, we image tibiae from Sost KO mice and their wild-type (WT) counterparts with high-resolution CT to examine whether lack of SCLEROSTIN influences the morphometric properties of lacunae and vascular canal porosity relating to osteocytes and vessels within cortical bone. Male Sost KO and WT mice (n = 6/group) were sacrificed at 12 weeks of age. Fixed tibiae were analyzed using microCT to examine cortical bone mass and architecture. Then, samples were imaged by using benchtop and synchrotron nano-computed tomography at the tibiofibular junction. Our data, consistent with previous studies show that, Sost deficiency leads to significant enhancement of bone mass by cortical thickening and bigger cross-sectional area and we find that this occurs without modifications of tibial ellipticity, a measure of bone shape. In addition, our data show that there are no significant differences in any lacunar or vascular morphometric or geometric parameters between Sost KO mouse tibia and WT counterparts. We, therefore, conclude that the significant

Journal article

De Souza R, Javaheri B, Collinson RS, Chenu C, Shefelbine SJ, Lee PD, Pitsillides AAet al., 2017, Prolonging disuse in aged mice amplifies cortical but not trabecular bones' response to mechanical loading, JOURNAL OF MUSCULOSKELETAL & NEURONAL INTERACTIONS, Vol: 17, Pages: 218-225, ISSN: 1108-7161

Objective:Short-term neurectomy-induced disuse (SN) has been shown to restore load responses in aged mice. We examined whether this restoration was further enhanced in both cortical and trabecular bone by simply extending the SN.Methods:Following load: strain calibration, tibiae in female C57BL/J6 mice at 8, 14 and 20 weeks and 18 months (n=8/group) were loaded and bone changes measured. Effects of long-term SN examined in twenty-six 18 months-old mice, neurectomised for 5 or 100 days with/without subsequent loading. Cortical and trabecular responses were measured histomorphometrically or by micro-computed tomography.Results:Loading increased new cortical bone formation, elevating cross-sectional area in 8, 14 and 20 week-old (p <0.05), but not 18 month-old aged mice. Histomorphometry showed that short-term SN reinstated load-responses in aged mice, with significant 33% and 117% increases in bone accrual at 47% and 37%, but not 27% of tibia length. Cortical responses to loading was heightened and widespread, now evident at all locations, following prolonged SN (108, 167 and 98% at 47, 37 and 27% of tibial length, respectively). In contrast, loading failed to modify trabecular bone mass or architecture.Conclusions:Mechanoadaptation become deficient with ageing and prolonging disuse amplifies this response in cortical but not trabecular bone.

Journal article

Kazantsev D, Guo E, Phillion AB, Withers PJ, Lee PDet al., 2017, Model-based iterative reconstruction using higher-order regularization of dynamic synchrotron data, MEASUREMENT SCIENCE AND TECHNOLOGY, Vol: 28, ISSN: 0957-0233

We present a novel iterative reconstruction method applied to in situ x-ray synchrotron tomographic data of dendrite formation during the solidification of magnesium alloy. Frequently, fast dynamic imaging projection data are undersampled, noisy, of poor contrast and can contain various acquisition artifacts. Direct reconstruction methods are not suitable and iterative reconstruction techniques must be adapted to the existing data features. Normally, an accurate modelling of the objective function can guarantee a better reconstruction. In this work, we design a special cost function where the data fidelity term is based on the Group-Huber functional to minimize ring artifacts and the regularization term is a higher-order variational penalty. We show that the total variation penalty is unsuitable for some cases and higher-order regularization functionals can ensure a better fit to the expected properties of the data. Additionally, we highlight the importance of 3D regularization over 2D for the problematic data. The proposed method shows a promising performance dealing with angular undersampled noisy dynamic data with ring artifacts.

Journal article

Reyes F, Lin Q, Udoudo O, Dodds C, Lee PD, Neethling Set al., 2017, Calibrated X-ray micro-tomography for mineral ore quantification, Minerals Engineering, Vol: 110, Pages: 122-130, ISSN: 0892-6875

Scanning Electron Microscopy (SEM) based assessments are the most widely used and trusted imaging technique for mineral ore quantification. X-ray micro tomography (XMT) is a more recent addition to the mineralogy toolbox, but with the potential to extend the measurement capabilities into the three dimensional (3D) assessment of properties such as mineral liberation, grain size and textural characteristics. In addition, unlike SEM based assessments which require the samples to be sectioned, XMT is non-invasive and non-destructive. The disadvantage of XMT, is that the mineralogy must be inferred from the X-ray attenuation measurements, which can make it hard to distinguish from one another, whereas SEM when coupled with Energy-Dispersive X-ray Spectroscopy (EDX) provides elemental compositions and thus a more direct method for distinguishing different minerals. A new methodology that combines both methods at the mineral grain level is presented. The rock particles used to test the method were initially imaged in 3D using XMT followed by sectioning and the 2D imaging of the slices using SEM-EDX. An algorithm was developed that allowed the mineral grains in the 2D slice to be matched with their 3D equivalents in the XMT based images. As the mineralogy of the grains from the SEM images can be matched to a range of X-ray attenuations, this allows minerals which have similar attenuations to one another to be distinguished, with the level of uncertainty in the classification quantified. In addition, the methodology allowed for the estimation of the level of uncertainty in the quantification of grain size by XMT, the assessment of stereological effects in SEM 2D images and ultimately obtaining a simplified 3D mineral map from low energy XMT images. Copper sulphide ore fragments, with chalcopyrite and pyrite as the main sulphide minerals, were used to demonstrate the effectiveness of this procedure.

Journal article

Ma L, Taylor KG, Dowey PJ, Courtois L, Gholinia A, Lee PDet al., 2017, Multi-scale 3D characterisation of porosity and organic matter in shales with variable TOC content and thermal maturity: Examples from the Lublin and Baltic Basins, Poland and Lithuania, International Journal of Coal Geology, Vol: 180, Pages: 100-112, ISSN: 0166-5162

Understanding the distribution of pores and organic matter with varying organic matter concentrations and maturity is essential to understanding fluid flow in shale systems. Analysis of samples with low, medium, and high total organic carbon (TOC) and varying maturities (gas-mature and oil-mature) enables the impact of both organic matter concentrations and thermal maturation on organic matter porosity to be examined. Three gas-mature samples of varying TOC (Lublin Basin) and one oil-mature sample (Baltic Basin), both with similar mineral compositions, were selected from the same formation. Samples were imaged in 3D over four orders of magnitudes (pixel sizes from 44 μm to 5 nm). A combination of X-ray computed tomography (XCT) and Focus Ion Beam Scanning Electron Microscopy (FIB-SEM) enabled the morphologic and topological characteristics of minerals, organic matter and pores to be imaged and quantified.In the studied samples, organic matter primarily has two geometries: lamellar masses (length: 1–100 μm, thickness: 0.5–2.0 μm) and discrete spheroidal particles (0.5–20.0 μm). Organic matter forms an inter-connected network where it exceeds a concentration between 6 and 18 wt%.Different pore types have different diameters and total pore volumes: inter-mineral pores (0.2 μm, 10–94%), organic interface pores (0.2 μm, 2–77%), intra-organic pores (0.05 μm, 1–40%) and intra-mineral pores (0.05 μm diameter, 1–2% of total porosity). The major pore system in the studied shales is composed of inter-mineral pores which occur between clay mineral grains. TOC concentration influences the total volume of organic matter-related pores while maturity controls the presence of intra-organic pores. The study improves the understanding of the relationship of organic matter concentrations, maturity and pore systems in shales. This study characterises porosity and organic matter distributions in 3D; it also improves the un

Journal article

nommeots-nomm A, lee PD, Jones JR, 2017, Direct ink writing of highly bioactive glasses, Journal of the European Ceramic Society, Vol: 28, Pages: 937-944, ISSN: 0955-2219

Direct ink writing (DIW) or Robocasting, is an additive manufacturing technique that offers the opportunity to create patient specific bioactive glass scaffolds and high strength scaffolds for bone repair. The original 45S5 Bioglass® composition crystallises during sintering and until now, robocast glass scaffolds contained at least 51.9 mol% SiO2 or B2O3 to maintain their amorphous structure. Here, ICIE16 and PSrBG compositions, containing <50 mol% SiO2, giving silicate network connectivity close to that of 45S5, were robocast and compared to 13–93 composition. Results showed Pluronic F-127 can be used as a universal binder regardless of glass reactivity and that particle size distribution affected the ink “printability”. Scaffolds with interconnects of 150 μm (41–43% porosity) had compressive strengths of 32–48 MPa, depending on the glass composition. Robocast scaffolds from these highly reactive bioactive glasses promise greatly improved bone regeneration rates compared with existing bioactive glass scaffolds.

Journal article

Javaheri B, Poulet B, Aljazzar A, de Souza R, Piles M, Hopkinson M, Shervill E, Pollard A, Chan B, Chang Y-M, Orriss IR, Lee PD, Pitsillides AAet al., 2017, Stable sulforaphane protects against gait anomalies and modifies bone microarchitecture in the spontaneous STR/Ort model of osteoarthritis, BONE, Vol: 103, Pages: 308-317, ISSN: 8756-3282

Osteoarthritis (OA), affecting joints and bone, causes physical gait disability with huge socio-economic burden; treatment remains palliative. Roles for antioxidants in protecting against such chronic disorders have been examined previously. Sulforaphane is a naturally occurring antioxidant. Herein, we explore whether SFX-01®, a stable synthetic form of sulforaphane, modifies gait, bone architecture and slows/reverses articular cartilage destruction in a spontaneous OA model in STR/Ort mice. Sixteen mice (n = 8/group) were orally treated for 3 months with either 100 mg/kg SFX-01® or vehicle. Gait was recorded, tibiae were microCT scanned and analysed. OA lesion severity was graded histologically. The effect of SFX-01® on bone turnover markers in vivo was complemented by in vitro bone formation and resorption assays. Analysis revealed development of OA-related gait asymmetry in vehicle-treated STR/Ort mice, which did not emerge in SFX-01®-treated mice. We found significant improvements in trabecular and cortical bone. Despite these marked improvements, we found that histologically-graded OA severity in articular cartilage was unmodified in treated mice. These changes are also reflected in anabolic and anti-catabolic actions of SFX-01® treatment as reflected by alteration in serum markers as well as changes in primary osteoblast and osteoclast-like cells in vitro. We report that SFX-01® improves bone microarchitecture in vivo, produces corresponding changes in bone cell behaviour in vitro and leads to greater symmetry in gait, without marked effects on cartilage lesion severity in STR/Ort osteoarthritic mice. Our findings support both osteotrophic roles and novel beneficial gait effects for SFX-01® in this model of spontaneous OA.

Journal article

Fauchille AL, Ma L, Rutter E, Chandler M, Lee PD, Taylor KGet al., 2017, An enhanced understanding of the Basinal Bowland shale in Lancashire (UK), through microtextural and mineralogical observations, MARINE AND PETROLEUM GEOLOGY, Vol: 86, Pages: 1374-1390, ISSN: 0264-8172

Variability in the Lower Bowland shale microstructure is investigated here, for the first time, from the centimetre to the micrometre scale using optical and scanning electron microscopy (OM, SEM), X-Ray Diffraction (XRD) and Total Organic Carbon content (TOC) measurements. A significant range of microtextures, organic-matter particles and fracture styles was observed in rocks of the Lower Bowland shale, together with the underlying Pendleside Limestone and Worston Shale formations encountered the Preese Hall-1 Borehole, Lancashire, UK. Four micro-texture types were identified: unlaminated quartz-rich mudstone; interlaminated quartz- and pyrite-rich mudstone; laminated quartz and pyrite-rich mudstone; and weakly-interlaminated calcite-rich mudstone. Organic matter particles are classified into four types depending on their size, shape and location: multi-micrometre particles with and without macropores: micrometre-size particles in cement and between clay minerals; multi-micrometre layers; and organic matter in large pores. Fractures are categorized into carbonate-sealed fractures; bitumen-bearing fractures; resin-filled fractures; and empty fractures. We propose that during thermal maturation, horizontal bitumen-fractures were formed by overpressuring, stress relaxation, compaction and erosional offloading, whereas vertical bitumen-bearing, resin-filled and empty fractures may have been influenced by weak vertical joints generated during the previous period of veining. For the majority of samples, the high TOC (>2 wt%), low clay content (<20 wt%), high proportion of quartz (>50 wt%) and the presence of a multi-scale fracture network support the increasing interest in the Bowland Shale as a potentially exploitable oil and gas source. The microtextural observations made in this study highlight preliminary evidence of fluid passage or circulation in the Bowland Shale sequence during burial.

Journal article

Taiwo OO, Finegan DP, Paz-Garcia JM, Eastwood DS, Bodey AJ, Rau C, Hall SA, Brett DJL, Lee PD, Shearing PRet al., 2017, Investigating the evolving microstructure of lithium metal electrodes in 3D using X-ray computed tomography, Physical Chemistry Chemical Physics, Vol: 19, Pages: 22111-22120, ISSN: 1463-9076

The growth of electrodeposited lithium microstructures on metallic lithium electrodes has prevented their use in rechargeable lithium batteries due to early performance degradation and safety implications. Understanding the evolution of lithium microstructures during battery operation is crucial for the development of an effective and safe rechargeable lithium-metal battery. This study employs both synchrotron and laboratory X-ray computed tomography to investigate the morphological evolution of the surface of metallic lithium electrodes during a single cell discharge and over numerous cycles, respectively. The formation of surface pits and the growth of mossy lithium deposits through the separator layer are characterised in three-dimensions. This has provided insight into the microstructural evolution of lithium-metal electrodes during rechargeable battery operation, and further understanding of the importance of separator architecture in mitigating lithium dendrite growth.

Journal article

Kao A, Cai B, Lee PD, Pericleous Ket al., 2017, The effects of Thermoelectric Magnetohydrodynamics in directional solidification under a transverse magnetic field, 5th European Conference for Crystal Growth (ECCG), Publisher: Elsevier, Pages: 270-274, ISSN: 1873-5002

The mechanism of macrosegregation and modification to dendrite size and spacing from a transverse magnetic field has been modelled through direct numerical simulation. The primary driver for this mechanism was identified as a strong Lorentz force formed in the interdendritic region, which leads to a large scale flow circulation. The microstructure evolution is modified by convective transport of solute and the predicted morphological features compare favourably to experimental data in the literature. The numerical results also give an insight into the magnitude of flow velocities within the interdendritic region.

Conference paper

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