Constitutive modelling of plastic deformation and damage in anisotropic high-purity titanium and validation using ex-situ and in-situ tomography data

The results on investigations of mechanical properties of high-purity titanium with grains ranging from tens of nanometers up to a few micrometers subjected to uniaxial tension, compression and microindenting are presented. Different structural states in high-purity titanium were formed by severe plastic deformation according to the scheme «upsetting – extrusion – drawing» in combination with annealing at temperatures of 250–550° C and quasi-hydrostatic extrusion at room and liquid nitrogen temperatures. The values of yield strengths and microhardness for samples of high-purity titanium with grains of different sizes are determined. It was shown that the combination of severe plastic deformation with cryogenic quasi-hydrostatic extrusion allowed to create high-purity nanocrystalline titanium with high mechanical properties. The obtained experimental data were analyzed for the implementation of the Hall-Petch relation and discrepancy between the values of yield strengths in tension and compression (strength differential or S-D effect). Satisfactory fulfillment of the Hall-Petch relation for high-purity titanium in the whole range of the studied grain size values was shown and a noticeable difference in the yield values for compression and tension was found. The values of the coefficients in the Hall-Petch equation for deformation by tension, compression and microindenting were determined. These coefficients are noticeably lower than the corresponding values for the industrial grades of titanium, i.e. in high-purity titanium, the grain boundaries are weaker barriers for moving dislocations than in the industrial titanium, whose boundaries are enriched with impurities. The features of the acoustic waves emission during compression of samples in various structural states were studied. It was concluded that the deformation of titanium in all the investigated structural states was carried out by dislocation slip.

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Bacterial Cellulose as a Versatile Platform for Research and Development of Biomedical Materials

Processes ◽

10.3390/pr8050624 ◽

2020 ◽

Vol 8 (5) ◽

pp. 624 ◽

Cited By ~ 6

Author(s):

Selestina Gorgieva

Keyword(s):

Bacterial Cellulose ◽

High Purity ◽

Antimicrobial Properties ◽

Wound Dressings ◽

Ex Situ ◽

Native Form ◽

Multifunctional Compounds ◽

Ultra High Purity ◽

Cell Affinity

The unique pool of features found in intracellular and extracellular bacterial biopolymers attracts a lot of research, with bacterial cellulose (BC) being one of the most versatile and common. BC is an exopolysaccharide consisting solely of cellulose, and the variation in the production process can vary its shape or even its composition when compounding is applied in situ. Together with ex situ modification pathways, including specialised polymers, particles or exclusively functional groups, BC provides a robust platform that yields complex multifunctional compounds that go far beyond ultra-high purity, intrinsic hydrophilicity, mechanical strength and biocompatibility to introduce bioactive, (pH, thermal, electro) responsive, conductive and ‘smart’ properties. This review summarises the research outcomes in BC-medical applications, focusing mainly on data from the past decade (i.e., 2010–2020), with special emphasis on BC nanocomposites as materials and devices applicable in medicine. The high purity and unique structural/mechanical features, in addition to its capacity to closely adhere to irregular skin surfaces, skin tolerance, and demonstrated efficacy in wound healing, all stand as valuable attributes advantageous in topical drug delivery. Numerous studies prove BC compatibility with various human cells, with modifications even improving cell affinity and viability. Even BC represents a physical barrier that can reduce the penetration of bacteria into the tissue, but in its native form does not exhibit antimicrobial properties, therefore carious modifications have been made or specific compounds added to confer antimicrobial or anti-inflammatory properties. Progress in the use of BC-compounds as wound dressings, vascular grafts, and scaffolds for the treatment of cartilage, bone and osteochondral defects, the role as a basement membrane in blood-brain barrier models and many more are discussed to particular extent, emphasising the need for BC compounding to meet specific requirements.

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Neutron Diffraction and Acoustic Emission Study of Mg-Al-Sr Alloy Reinforced with Short Saffil® Fibers Deformed in Compression

Materials Science Forum ◽

10.4028/www.scientific.net/msf.777.92 ◽

2014 ◽

Vol 777 ◽

pp. 92-98 ◽

Cited By ~ 2

Author(s):

Gergely Farkas ◽

Kristián Máthis ◽

Petr Lukáš ◽

Jan Pilch ◽

Miroslav Vrána ◽

...

Keyword(s):

Residual Stress ◽

Plastic Deformation ◽

Acoustic Emission ◽

Neutron Diffraction ◽

Residual Stresses ◽

Deformation Mechanisms ◽

Ex Situ ◽

The Matrix ◽

Main Deformation

Neutron diffraction method has been applied in theex-situinvestigation of the residual stresses in Mg-5wt.%Al-1 wt.%Sr (AJ51) magnesium alloy reinforced with short Saffil® fibers deformed in compression at room temperature. The residual stresses were measured in the axial and radial directions with respect to the load direction. It is shown that in the initial state the tensile stress is present in the matrix phase. Thein-situacoustic emission measurements were performed with the aim to reveal the main deformation mechanisms operating in the particular stages of the plastic deformation. Ex-situ neutron diffractions experiments showed that the tensile axial residual stress in the matrix increases with increasing plastic deformation while the radial residual stress decreases. In situ acoustic emission measurements indicate that the main deformation mechanisms are twinning and glide of bigger dislocation ensembles in the early stages of the compressive deformation while the fibers breakage was observed in the vicinity of the maximum stress.

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In situ TEM observation of tensile deformation in high-purity titanium after a single compression stroke

Scripta Metallurgica ◽

10.1016/0036-9748(89)90450-x ◽

1989 ◽

Vol 23 (4) ◽

pp. 553-556 ◽

Cited By ~ 2

Author(s):

Zhang Jieping ◽

Gu Haicheng ◽

Zhou Huiju ◽

Campbell Laird

Keyword(s):

High Purity ◽

Tensile Deformation ◽

In Situ Tem ◽

Compression Stroke ◽

Purity Titanium

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An in situ and ex situ TEM study of the formation of thin cobalt silicide films by molecular beam epitaxy on the silicon (100) surface

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s042482010010648x ◽

1988 ◽

Vol 46 ◽

pp. 884-885

Author(s):

D. Loretto ◽

J. M. Gibson ◽

S. M. Yalisove ◽

R. T. Tung

Keyword(s):

Molecular Beam Epitaxy ◽

Molecular Beam ◽

Defect Density ◽

High Vacuum ◽

Ultra High Vacuum ◽

Ex Situ ◽

Metal Base ◽

In Situ Experiments ◽

Potential Applications

The cobalt disilicide/silicon system has potential applications as a metal-base and as a permeable-base transistor. Although thin, low defect density, films of CoSi2 on Si(111) have been successfully grown, there are reasons to believe that Si(100)/CoSi2 may be better suited to the transmission of electrons at the silicon/silicide interface than Si(111)/CoSi2. A TEM study of the formation of CoSi2 on Si(100) is therefore being conducted. We have previously reported TEM observations on Si(111)/CoSi2 grown both in situ, in an ultra high vacuum (UHV) TEM and ex situ, in a conventional Molecular Beam Epitaxy system.The procedures used for the MBE growth have been described elsewhere. In situ experiments were performed in a JEOL 200CX electron microscope, extensively modified to give a vacuum of better than 10-9 T in the specimen region and the capacity to do in situ sample heating and deposition. Cobalt was deposited onto clean Si(100) samples by thermal evaporation from cobalt-coated Ta filaments.

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The use of transmission and analytical electron microscopy in studying reactions and phase transformations in thin film

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100150046 ◽

1993 ◽

Vol 51 ◽

pp. 842-843

Author(s):

K. Barmak

Keyword(s):

Thin Film ◽

Thin Films ◽

Phase Transformations ◽

Analytical Electron Microscopy ◽

Ex Situ ◽

Multilayer Thin Films ◽

Absolute Concentration ◽

Analytical Electron ◽

Deposition Step

Generally, processing of thin films involves several annealing steps in addition to the deposition step. During the annealing steps, diffusion, transformations and reactions take place. In this paper, examples of the use of TEM and AEM for ex situ and in situ studies of reactions and phase transformations in thin films will be presented.The ex situ studies were carried out on Nb/Al multilayer thin films annealed to different stages of reaction. Figure 1 shows a multilayer with dNb = 383 and dAl = 117 nm annealed at 750°C for 4 hours. As can be seen in the micrograph, there are four phases, Nb/Nb3-xAl/Nb2-xAl/NbAl3, present in the film at this stage of the reaction. The composition of each of the four regions marked 1-4 was obtained by EDX analysis. The absolute concentration in each region could not be determined due to the lack of thickness and geometry parameters that were required to make the necessary absorption and fluorescence corrections.

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Transmission Electron Microscopy of Epitaxial silicides grown by ultra high vacuum deposition

Proceedings, annual meeting, Electron Microscopy Society of America ◽

10.1017/s0424820100154287 ◽

1989 ◽

Vol 47 ◽

pp. 462-463

Author(s):

D. Loretto ◽

J. M. Gibson ◽

S. M. Yalisove

Keyword(s):

Electron Microscopy ◽

Transmission Electron Microscopy ◽

Electron Diffraction ◽

High Vacuum ◽

High Energy ◽

Energy Electron ◽

Ultra High Vacuum ◽

Ex Situ ◽

Transmission Electron

The silicides CoSi2 and NiSi2 are both metallic with the fee flourite structure and lattice constants which are close to silicon (1.2% and 0.6% smaller at room temperature respectively) Consequently epitaxial cobalt and nickel disilicide can be grown on silicon. If these layers are formed by ultra high vacuum (UHV) deposition (also known as molecular beam epitaxy or MBE) their thickness can be controlled to within a few monolayers. Such ultrathin metal/silicon systems have many potential applications: for example electronic devices based on ballistic transport. They also provide a model system to study the properties of heterointerfaces. In this work we will discuss results obtained using in situ and ex situ transmission electron microscopy (TEM).In situ TEM is suited to the study of MBE growth for several reasons. It offers high spatial resolution and the ability to penetrate many monolayers of material. This is in contrast to the techniques which are usually employed for in situ measurements in MBE, for example low energy electron diffraction (LEED) and reflection high energy electron diffraction (RHEED), which are both sensitive to only a few monolayers at the surface.

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Atomic Layer Deposition of LiF and Lithium Ion Conducting (AlF3)(LiF)x Alloys Using Trimethylaluminum, Lithium Hexamethyldisilazide and Hydrogen Fluoride

10.26434/chemrxiv.5459653 ◽

2017 ◽

Author(s):

Younghee Lee ◽

Daniela M. Piper ◽

Andrew S. Cavanagh ◽

Matthias J. Young ◽

Se-Hee Lee ◽

...

Keyword(s):

Lithium Ion ◽

Atomic Layer ◽

Mass Gain ◽

Alloy Film ◽

Ex Situ ◽

X Ray ◽

Layer Deposition ◽

Ion Conducting ◽

Good Agreement

<div>Atomic layer deposition (ALD) of LiF and lithium ion conducting (AlF3)(LiF)x alloys was developed using trimethylaluminum, lithium hexamethyldisilazide (LiHMDS) and hydrogen fluoride derived from HF-pyridine solution. ALD of LiF was studied using in situ quartz crystal microbalance (QCM) and in situ quadrupole mass spectrometer (QMS) at reaction temperatures between 125°C and 250°C. A mass gain per cycle of 12 ng/(cm2 cycle) was obtained from QCM measurements at 150°C and decreased at higher temperatures. QMS detected FSi(CH3)3 as a reaction byproduct instead of HMDS at 150°C. LiF ALD showed self-limiting behavior. Ex situ measurements using X-ray reflectivity (XRR) and spectroscopic ellipsometry (SE) showed a growth rate of 0.5-0.6 Å/cycle, in good agreement with the in situ QCM measurements.</div><div>ALD of lithium ion conducting (AlF3)(LiF)x alloys was also demonstrated using in situ QCM and in situ QMS at reaction temperatures at 150°C A mass gain per sequence of 22 ng/(cm2 cycle) was obtained from QCM measurements at 150°C. Ex situ measurements using XRR and SE showed a linear growth rate of 0.9 Å/sequence, in good agreement with the in situ QCM measurements. Stoichiometry between AlF3 and LiF by QCM experiment was calculated to 1:2.8. XPS showed LiF film consist of lithium and fluorine. XPS also showed (AlF3)(LiF)x alloy consists of aluminum, lithium and fluorine. Carbon, oxygen, and nitrogen impurities were both below the detection limit of XPS. Grazing incidence X-ray diffraction (GIXRD) observed that LiF and (AlF3)(LiF)x alloy film have crystalline structures. Inductively coupled plasma mass spectrometry (ICP-MS) and ionic chromatography revealed atomic ratio of Li:F=1:1.1 and Al:Li:F=1:2.7: 5.4 for (AlF3)(LiF)x alloy film. These atomic ratios were consistent with the calculation from QCM experiments. Finally, lithium ion conductivity (AlF3)(LiF)x alloy film was measured as σ = 7.5 × 10-6 S/cm.</div>

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A New Method of Wafer Level Plan View TEM Sample Preparation by DualBeam

ISTFA 2008: Conference Proceedings from the 34th International Symposium for Testing and Failure Analysis ◽

10.31399/asm.cp.istfa2008p0168 ◽

2008 ◽

Author(s):

Hyoung H. Kang ◽

Michael A. Gribelyuk ◽

Oliver D. Patterson ◽

Steven B. Herschbein ◽

Corey Senowitz

Keyword(s):

Sample Preparation ◽

Ex Situ ◽

Wafer Level ◽

Cross Sectional ◽

Plan View ◽

Manufacturing Line ◽

Transmission Electron ◽

Thin Lamella ◽

Preparation Techniques

Abstract Cross-sectional style transmission electron microscopy (TEM) sample preparation techniques by DualBeam (SEM/FIB) systems are widely used in both laboratory and manufacturing lines with either in-situ or ex-situ lift out methods. By contrast, however, the plan view TEM sample has only been prepared in the laboratory environment, and only after breaking the wafer. This paper introduces a novel methodology for in-line, plan view TEM sample preparation at the 300mm wafer level that does not require breaking the wafer. It also presents the benefit of the technique on electrically short defects. The methodology of thin lamella TEM sample preparation for plan view work in two different tool configurations is also presented. The detailed procedure of thin lamella sample preparation is also described. In-line, full wafer plan view (S)TEM provides a quick turn around solution for defect analysis in the manufacturing line.

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