Ingenieurwissenschaften und zugeordnete Tätigkeiten
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- Nanoparticle (11)
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This study presents the synthesis and characterization of zwitterionic core–shell hybrid nanoparticles consisting of a core of iron oxide multicore nanoparticles (MCNPs, γ-Fe2O3) and a shell of sultonated poly(2-vinylpyridine-grad-acrylic acid) copolymers. The gradient copolymers are prepared by reversible addition fragmentation chain transfer polymerization of 2-vinylpyridine (2VP), followed by the addition of tert-butyl acrylate and subsequent hydrolysis. Grafting of P(2VP-grad-AA) onto MCNP results in P(2VP-grad-AA)@MCNP, followed by quaternization using 1,3-propanesultone-leading to P(2VPS-grad-AA)@MCNP with a zwitterionic shell. The resulting particles are characterized by transmission electron microscopy, dynamic light scattering, and thermogravimetric analysis measurements, showing particle diameters of ≈70–90 nm and an overall content of the copolymer shell of ≈10%. Turbidity measurements indicate increased stability toward secondary aggregation after coating if compared to the pristine MCNP and additional cytotoxicity tests do not reveal any significant influence on cell viability.
X-ray tomography characterisation of lattice structures processed by selective electron beam melting
(2017)
Metallic lattice structures intentionally contain open porosity; however, they can also contain unwanted closed porosity within the structural members. The entrained porosity and defects within three different geometries of Ti-6Al-4V lattices, fabricated by Selective Electron Beam Melting (SEBM), is assessed from X-ray computed tomography (CT) scans. The results suggest that horizontal struts that are built upon loose powder show particularly high (~20 x 10⁻³ vol %) levels of pores, as do nodes at which many (in our case 24) struts meet. On the other hand, for struts more closely aligned (0° to 54°) to the build direction, the fraction of porosity appears to be much lower (~0.17 x 10⁻³%) arising mainly from pores contained within the original atomised powder particles.
High-strength steels with yield strengths ≥ 690 MPa are becoming increasingly significant for modern steel constructions. Both quenched and tempered (QT) high-strength steels and steels produced by the thermo-mechanically controlled process (TMCP) are currently available. TMCP-steels are usually provided with a typical mill scale. Apart from the manufacturing process these steels differ also in their chemical composition. The influence of these differences are investigated here with focus on the residual stresses formed during TIG welding. Bead on plate welds have shown characteristic residual stress distributions depending on the type of steel as well as on the heat input and preheat temperature. The following work demonstrates that the fluid flow, induced by the elements present in the mill scale, leads to a deeper penetration of the material. This can also lead to increased residual stresses in the surface of the weld and the HAZ. Furthermore, higher heat input and preheat temperature can induce higher tensile residual stresses − which are evident in the present study.
We present a first direct measurement of the temperature during milling combined with in situ Raman spectroscopy monitoring. The data reveal a low temperature increase due to the mechanical impact and clear temperature increases as a consequence of the reaction heat. Based on the data, temperature rises as postulated in the magma plasma and hot spot theory can be excluded for soft matter milling syntheses.
The current review focuses on vesicles obtained from the self-assembly of two types of dendritic macromolecules, namely amphiphilic Janus dendrimers (forming dendrimersomes) and amphiphilic dumbbells. In the first part, we will present some synthetic strategies and the various building blocks that can be used to obtain dendritic-based macromolecules, thereby showing their structural versatility. We put our focus on amphiphilic Janus dendrimers and amphiphilic dumbbells that form vesicles in water but we also encompass vesicles formed thereof in organic solvents. The second part of this review deals with the production methods of these vesicles at the nanoscale but also at the microscale. Furthermore, the influence of various parameters (intrinsic to the amphiphilic JD and extrinsic—from the environment) on the type of vesicle formed will be discussed. In the third part, we will review the numerous biomedical applications of these vesicles of nano- or micron-size.
Fracture mechanics based component design requires appropriate fracture mechanics toughness data with respect to both, loading rate as well as test temperature. Taking high-rate loading into account such as with accidental scenarios, different standards such as ASTM E 1820 or BS 7448-3 provide some information on dynamic fracture mechanics testing. Nevertheless, the designations differ so that a validation of the own material specific test method used for dynamic R-curve determination is mandatory. In order to address this for ductile cast iron materials an experimental method for the reliable determination of dynamic J-integral crack resistance curves at -40 °C following the multiple specimen approach has been established and validated. The experimental concept offers some additional valuable features. Single values of dynamic crack initiation toughness can be determined using a single specimen technique based on crack sensors. Furthermore, an experimentally independent method is provided according to which CTOD δ5 R-curves can be established. The focus of the present paper is on the validation of the experimental low blow technique using a drop tower test system.
A drop tower test system was developed and set up to perform low blow tests at temperatures down to -40 °C. The system allows for a variation of the impact mass and height and was optimized for testing of ductile cast iron at stress intensity rates from approximately 5∙10⁴ to 3∙10⁵ MPa√ms⁻¹. This range of loading rate is characteristic for instance with crash scenarios of heavy sectioned DCI casks for radioactive materials. In order to address characteristic challenges of impact tests (test duration of microseconds up to milliseconds, inertial effects, signal oscillations), an appropriate full bridge strain gage method for the measurement of force directly on the specimen as well as a non-contact measurement of load line displacement using an optical extensometer have been developed and validated.
The low blow test requires either to prevent bouncing strikes of the hammer by using the stop block technique or to catch the hammer after its first strike. Both options are not part of the experimental concept and setup which have been realized here. The paper describes investigations which have been performed in order to make sure that bouncing strikes of the hammer do not cause additional crack extension in the specimen. This is necessary to ensure a unique relation between the work done and the achieved crack extension. The investigations covered the analysis of limit loads of the specimen with respect to the measured force. The measured stiffness of the specimen was assessed and signals of crack sensors were analyzed. Furthermore, an analysis of the mechanical behavior of the loading system and the specimen by optical observation was performed. Corresponding results are discussed in the paper. It had finally been proven that additional crack extension in the specimen due to bouncing strikes of the hammer is not to be expected under the given conditions of test setup, material and loading. It can be seen as a major experimental advantage that the striker does not have to be catched after the low blow test.
Ellipsometry is a useful tool for studying the optical properties of thin films such as photovoltaic devices. We employ Müller matrix ellipsometry to study the thin film photovoltaic material copper indium gallium selenide Cu(In,Ga) Se2 (CIGS), a commercially relevant material with high energy conversion efficiency. Confocal microscopy reveals an rms roughness of 68 nm, which greatly affects the ellipsometry data. Rayleigh-Rice theory is employed to account for the optical properties of the surface roughness in the ellipsometry experiment, and a library search method is used to compare Müller parameters calculated for various CIGS compositions, to the measured data. The Müller parameters calculated with the Rayleigh-Rice model are found to correspond well with the measured data, and a surface roughness of 37nm and a correlation length of 125nm are extracted.
A combination of nanosized dielectric relaxation (BDS) and thermal spectroscopy (SHS) was utilized to characterize the dynamics of thin films of Poly(vinyl methyl ether) (PVME) (thicknesses: 7 nm – 160 nm). For the BDS measurements, a recently designed nano-structured electrode system is employed. A thin film is spin-coated on an ultra-flat highly conductive silicon wafer serving as the bottom electrode. As top electrode, a highly conductive wafer with non-conducting nanostructured SiO2 nano-spacers with heights of 35 nm or 70 nm is assembled on the bottom electrode. This procedure results in thin supported films with a free polymer/air interface. The BDS measurements show two relaxation processes, which are analyzed unambiguously for thicknesses smaller than 50 nm. The relaxation rates of both processes have different temperature dependencies. One process coincidences in its position and temperature dependence with the glassy dynamics of bulk PVME and is ascribed to the dynamic glass transition of a bulk-like layer in the middle of the film. The relaxation rates were found to be thickness independent as confirmed by SHS. Unexpectedly, the relaxation rates of the second process obey an Arrhenius-like temperature dependence. This process was not observed by SHS and was related to the constrained fluctuations in a layer, which is irreversibly adsorbed at the substrate with a heterogeneous structure. Its molecular fluctuations undergo a confinement effect resulting in the localization of the segmental dynamics. To our knowledge, this is the first report on the molecular dynamics of an adsorbed layer in thin films.
Unusual Corrosion Behavior of 1.4542 Exposed a Laboratory Saline Aquifer Water CCS-Environment
(2017)
Differently heat treated coupons of 1.4542 were kept at T=60 °C and ambient pressure as well as p=100 bar for 700 h - 8000 h in an a) water saturated supercritical CO2 and b) CO2-saturated synthetic aquifer environment similar to on-shore CCS-sites in the Northern German Basin. Surface corrosion layers are homogeneous but unusually discontinuously ellipsoidal. After 8000 h at 100 bar maximum corrosion rate in the liquid phase is approximately 0.014 mm/year, with normalizing providing best corrosion resistance and approximately 0.003 mm/year in the supercritical phase where hardening+tempering at 670 °C leads to lowest corrosion rates.