Evolution of local misorientations in the γ/γ'-microstructure of single crystal superalloys during creep studied with the rotation vector baseline (RVB) EBSD method.

The present work uses the rotation vector baseline electron back scatter orientation imaging method (RVB-EBSD) to study the evolution of small misorientations between the γ- and γ'-phase in Ni-base single crystal superalloys (SXs) during creep. For this purpose, two material states of the SX ERBO1 (CMSX4 type) were characterized after creep deformation at 850°C and 600 MPa to final strains of 1% and 2%. Obtaining reliable phase boundary misorientation (PBM), kernel average misorientation (KAM) and orientation spread (OS) data represents a challenge for electron backscatter diffraction (EBSD), not only because the method operates at its limits of lateral and angular resolution, but also because it is difficult to differentiate between the two phases merely based on Kikuchi diffraction. The two phases differ in chemical composition which gives rise to different EBSD background intensities. These can be exploited to differentiate between the two phases. In the present work, crystallographic and chemical information are combined to demonstrate that orientation imaging can be used to document the formation of dislocation networks at γ/γ'-interfaces and the filling of γ-channels by dislocations. These findings are in good agreement with reference results from diffraction contrast scanning transmission electron microscopy. It is also shown that misorientations evolve between small groups of equally oriented γ/γ'-neighborhoods, on a size scale above characteristic γ/γ'-dimensions (>0.5 µm) and below distances associated with dendritic mosaicity (<200 µm). The methodological aspects as well as the new material specific results are discussed in the light of previous work published in the literature. RESEARCH HIGHLIGHTS: Microstructure evolution during [001] tensile creep of Ni-based single-crystalline alloy. Application of RVB-EBSD technique, focused on angular misorientations between γ/γ' phases, with accuracy of 0.01°. Separation of γ/γ' phases using experimental post-processing of raw EBSD data.

Benchmark dataset of the effect of grain size on strength in the single-phase FCC CrCoNi medium entropy alloy.

This data article presents the microstructural data as well as the mechanical properties of the CrCoNi medium-entropy alloy (MEA). The data presented in this article are related to the research article entitled "Analysis of strengthening due to grain boundaries and annealing twin boundaries in the CrCoNi medium-entropy alloy", see Ref. Schneider et al., 2019. This article can be referred to for the analysis and interpretation of the data, as well as their comparison to other datasets in literature. Microstructural data available in the present paper are backscattered electron micrographs for sixteen different grain sizes. Also available are pdf reports of grain size analysis (annealing twin boundaries were neglected) and crystallite sizes (including annealing twin boundaries) as well as data describing the number of annealing twin boundaries per grain (n), corresponding Taylor factors (M) and average annealing twin thicknesses (t). Additionally, raw data of stress-strain curves at five different temperatures [77 K, 293 K, 473 K, 673 K and 873 K] are given for all sixteen grain sizes, which may be used for further research, e.g. data mining, machine learning and other analytical methods. Mechanical data such as yield stresses (σ 0.2% ), Hall-Petch parameters (σ 0 and k y ) and critical boundary strengths (τ c ) are provided along with a 1D discrete dislocation dynamics (1-D DDD) simulation results concerning the different boundary strengths.

Ni-base superalloy single crystal (SX) mosaicity characterized by the Rotation Vector Base Line Electron Back Scatter Diffraction (RVB-EBSD) method.

In the present work we present the Rotation Vector Base Line Electron Back Scatter Diffraction (RVB-EBSD) method, a new correlative orientation imaging method for scanning electron microscopy (OIM/SEM). The RVB-EBSD method was developed to study crystal mosaicity in as-cast Ni-base superalloy single crystals (SX). The technique allows to quantify small crystallographic deviation angles between individual dendrites and to interpret associated accommodation processes in terms of geometrically necessary dislocations (GNDs). The RVB-EBSD method was inspired by previous seminal approaches which use cross correlation EBSD procedures. It applies Gaussian band pass filtering to improve the quality of more than 500 000 experimental patterns. A rotation vector approximation and a correction procedure, which relies on a base line function, are used. The method moreover features a novel way of intuitive color coding which allows to easily appreciate essential features of crystal mosaicity. The present work describes the key elements of the method and shows examples which demonstrate its potential.

Bioactivity and electrochemical behavior of hydroxyapatite-silicon-multi walled carbon nano-tubes composite coatings synthesized by EPD on NiTi alloys in simulated body fluid.

In order to improve the surface bioactivity of NiTi bone implant and corrosion resistance, hydroxyapatite coating with addition of 20wt% silicon, 1wt% multi walled carbon nano-tubes and both of them were deposited on a NiTi substrate using a cathodic electrophoretic method. The apatite formation ability was estimated using immersion test in the simulated body fluid for 10days. The SEM images of the surface of coatings after immersion in simulated body fluid show that the presence of silicon in the hydroxyapatite coatings accelerates in vitro growth of apatite layer on the coatings. The Open-circuit potential and electrochemical impedance spectroscopy were measured to evaluate the electrochemical behavior of the coatings in the simulated body fluid at 37°C. The results indicate that the compact structure of hydroxyapatite-20wt% silicon and hydroxyapatite-20wt% silicon-1wt% multi walled carbon nano-tubes coatings could efficiently increase the corrosion resistance of NiTi substrate.

Advanced scanning transmission stereo electron microscopy of structural and functional engineering materials.

Stereo transmission electron microscopy (TEM) provides a 3D impression of the microstructure in a thin TEM foil. It allows to perform depth and TEM foil thickness measurements and to decide whether a microstructural feature lies inside of a thin foil or on its surface. It allows appreciating the true three-dimensional nature of dislocation configurations. In the present study we first review some basic elements of classical stereo TEM. We then show how the method can be extended by working in the scanning transmission electron microscope (STEM) mode of a modern analytical 200 kV TEM equipped with a field emission gun (FEG TEM) and a high angle annular dark field (HAADF) detector. We combine two micrographs of a stereo pair into one anaglyph. When viewed with special colored glasses the anaglyph provides a direct and realistic 3D impression of the microstructure. Three examples are provided which demonstrate the potential of this extended stereo TEM technique: a single crystal Ni-base superalloy, a 9% Chromium tempered martensite ferritic steel and a NiTi shape memory alloy. We consider the effect of camera length, show how foil thicknesses can be measured, and discuss the depth of focus and surface effects.

Cell type-specific responses of peripheral blood mononuclear cells to silver nanoparticles.

Silver nanoparticles (Ag-NP) are increasingly used in biomedical applications because of their remarkable antimicrobial activity. In biomedicine, Ag-NP are coated onto or embedded in wound dressings, surgical instruments and bone substitute biomaterials, such as silver-containing calcium phosphate cements. Free Ag-NP and silver ions are released from these coatings or after the degradation of a biomaterial, and may come into close contact with blood cells. Despite the widespread use of Ag-NP as an antimicrobial agent, there is a serious lack of information on the biological effects of Ag-NP on human blood cells. In this study, the uptake of Ag-NP by peripheral monocytes and lymphocytes (T-cells) was analyzed, and the influence of nanosilver on cell biological functions (proliferation, the expression of adhesion molecules, cytokine release and the generation of reactive oxygen species) was studied. After cell culture in the presence of monodispersed Ag-NP (5-30µgml(-1) silver concentration), agglomerates of nanoparticles were detected within monocytes (CD14+) but not in T-cells (CD3+) by light microscopy, flow cytometry and combined focused ion beam/scanning electron microscopy. The uptake rate of nanoparticles was concentration dependent, and the silver agglomerates were typically found in the cytoplasm. Furthermore, a concentration-dependent activation (e.g. an increased expression of adhesion molecule CD54) of monocytes at Ag-NP concentrations of 10-15µgml(-1) was observed, and cytotoxicity of Ag-NP-treated monocytes was observed at Ag-NP levels of 25µgml(-1) and higher. However, no modulation of T-cell proliferation was observed in the presence of Ag-NP. Taken together, our results provide the first evidence for a cell-type-specific uptake of Ag-NP by peripheral blood mononuclear cells (PBMC) and the resultant cellular responses after exposure.

Structural and magnetic characterization of self-assembled iron oxide nanoparticle arrays.

We report about a combined structural and magnetometric characterization of self-assembled magnetic nanoparticle arrays. Monodisperse iron oxide nanoparticles with a diameter of 20 nm were synthesized by thermal decomposition. The nanoparticle suspension was spin-coated on Si substrates to achieve self-organized arrays of particles and subsequently annealed at various conditions. The samples were characterized by x-ray diffraction, and bright and dark field high resolution transmission electron microscopy. The structural analysis is compared to magnetization measurements obtained by superconducting quantum interference device magnetometry. We can identify either multi-phase Fe(x)O/γ-Fe(2)O(3) or multi-phase Fe(x)O/Fe(3)O(4) nanoparticles. The Fe(x)O/γ-Fe(2)O(3) system shows a pronounced exchange bias effect which explains the peculiar magnetization data found for this system.

Can human mesenchymal stem cells survive on a NiTi implant material subjected to cyclic loading?

Nickel-titanium shape memory alloys (NiTi-SMAs) exhibit mechanical and chemical properties which make them attractive candidate materials for various types of biomedical applications. However, the high nickel content of NiTi-SMAs may result in adverse tissue reactions, especially when they are considered for load-bearing implants. It is generally assumed that a protective titanium oxide layer separates the metallic alloy from its environment and that this explains the good biocompatibility of NiTi. Cyclic loading may result in failure of the protective oxide layer. The scientific objective of this work was to find out whether cyclic dynamic strain, in a range relevant for orthopedic implants, diminishes the biocompatibility of NiTi-SMAs. In order to analyze the biocompatibility of NiTi-SMA surfaces subjected to cyclic loading, NiTi-SMA tensile specimens were preloaded with mesenchymal stem cells, transferred to a sterile cell culture system and fixed to the pull rods of a tensile testing machine. Eighty-six thousand and four hundred strain cycles at 2% pseudoelastic strain were performed for a period of 24 h or 7 days. Cytokines (IL-6, IL-8 and VEGF) and nickel ion release were determined within the cell culture medium. Adherent cells on the tensile specimens were stained with calcein-AM and propidium iodide to determine cell viability. Dynamic loading of the tensile specimens did not influence the viability of adherent human mesenchymal stem cells (hMSCs) after 24 h or 7 days compared with the non-strained control. Dynamic cycles of loading and unloading did not affect nickel ion release from the tensile specimens. The release of IL-6 from hMSCs cultured under dynamic conditions was significantly higher after mechanical load (873 pg ml(-1)) compared with static conditions (323 pg ml(-1)). The present work demonstrates that a new type of mechanical in vitro cell culture experiment can provide information which previously could only be obtained in large animal experiments.

Modification of the bilateral sagittal split osteotomy (BSSO) in a study using pig mandibles.

In a bilateral sagittal split osteotomy (BSSO) mechanical irritation of the inferior alveolar nerve (IAN) (e.g. by chiselling) should be avoided to prevent neural damage. A modification of the Obwegeser-Dal Pont operation technique was studied by splitting 100 pig mandibles ex vivo. An additional osteotomy at the caudal border of the mandible was used to facilitate the sagittal split by means of a locus of minor resistance. The chisel was inserted distal to the second molar and far away from the IAN. The mandible was split by torque. The modified technique reduced the required torque to split the mandible about 30% compared with the original technique (paired t-test, t(69)=-12.89; p<0.05). 75% of all mandibles split by the modified technique were classified as bad splits compared with 100% using the original technique using the same protocol without the additional osteotomy.

Uptake and intracellular distribution of silver nanoparticles in human mesenchymal stem cells.

Silver nanoparticles (Ag-NP) are widely used due to their well-known antibacterial effects. In medicine Ag-NP have found applications as wound dressings, surgical instruments and bone substitute biomaterials, e.g. silver-containing calcium phosphate cements. Depending on the coating technique, during resorption of a biomaterial Ag-NP may come into close contact with body tissues, including human mesenchymal stem cells (hMSC). Despite the widespread uses of Ag-NP, there is a serious lack of information concerning their biological effects on human cells. In this study the uptake of Ag-NP into hMSC has been analyzed and the intracellular distribution of Ag-NP after exposure determined. Non-agglomerated (dispersed) Ag-NP from the cell culture medium were detected as agglomerates of nanoparticles within the hMSC by combined focused ion beam/scanning electron microscopy. The silver agglomerates were typically located in the perinuclear region, as determined by light microscopy. Specific staining of cellular structures (endo-lysosomes, nuclei, Golgi complex and endoplasmatic reticulum) using fluorescent probes showed that the silver nanoparticles occurred mainly within endo-lysosomal structures, not in the cell nucleus, endoplasmic reticulum or Golgi complex. Quantitative determination of the uptake of Ag-NP by flow cytometry (scattergram analysis) revealed a concentration-dependent uptake of the particles which was significantly inhibited by chlorpromazine and wortmannin but not by nystatin, indicating clathrin-dependent endocytosis and macropinocytosis as the primary uptake mechanisms.

High-temperature dislocation plasticity in the single-crystal superalloy LEK94.

The evolution of the dislocation structure that forms during uniaxial creep deformation in the single-crystal superalloy LEK94 of low density and with Re additions was analysed using transmission electron microscopy. The material has a gamma/gamma'-microstructure consisting of gamma'-cubes (L12 phase, 80 vol.%) separated by thin gamma-channels (face-centred cubic). <100> tensile creep tests were performed at 980 and 1020 degrees C at stresses of 200 and 240 MPa. The microstructure was investigated at three characteristic stages of creep (directly after loading, at 5% strain and after rupture) to show the evolution of the dislocation structure during high-temperature creep. It was found that in the early stages of creep, a(0)/2<011> dislocations form within the gamma-channels. Later on, dislocation networks form and gamma' cutting processes with a(0)/<001> superdislocations are observed. The results are in line with observations made for other superalloy single crystals in the high-temperature low-stress creep regime.