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Nanotechnology at BAM
(2017)
High-strength steels are favoured materials in the industry for production of safe and sustainable structures. The main technology used for joining the components of such steel is fusion welding.
Steel alloy design concepts combined with advanced processing technologies have been extensively investigated during the development of High-Strength Low-Alloy (HSLA) steels. However, very few studies have addressed the issue of how various alloy designs, even with limited microalloy addition, can influence the properties of high-strength steel welds. In high-strength steel welding practices, the challenges regarding microstructure evolution and the resulting mechanical properties variation, are of great interest. The main focus is the debate regarding the role of microalloy elements on phase transformation and weld performance. Limited Heat Affected Zone (HAZ) softening and limited austenite grain coarsening are significant design essentials, but the primary goal is to ensure excellent toughness and tensile properties in the steel weld. To achieve this purpose, microalloy elements such as Ti, Nb, or V were intentionally added to modern high-strength steels. The focus of this work was to understand the mechanical properties of HSLA steels resulting from differences in alloy design after joining by modern welding processes.
To begin, three microalloyed S690QL steels (Nb, Ti, and Ti+V addition) were investigated. Optical microscopy confirmed that similar mixtures of tempered bainite and martensite predominated the parent microstructure in the three steels, different types of coarse microalloy precipitates were also visible. These precipitates were analysed by using a thermodynamic-based software and then identified by Transmission Electron Microscopy (TEM). Results of mechanical testing revealed that all three steels performed above the standard toughness and tensile strength values, but with varied yielding phenomena. During the welding operation, each of the three steels was joined by using the same filler material. The fused weld metal was influenced by the high dilution of microalloyed elements in the base metal, this was significantly pronounced during the modified spray arc welding technique. As a result, the Nb-containing steel exhibited sufficient amounts of alloy pick-up to transition the microstructure in the weld metal from acicular ferrite to bainite as cooling rate was increased, leading to reduced toughness. This was not observed with the other two steels.
A second focus was made on the microstructure Evolution and toughness properties of the coarse and fine grained HAZ as welding parameters changed. In order to characterise the microstructure and austenite grain growth behaviour, physical simulations were conducted. The microalloy precipitates were found to be a dominant factor restricting the austenite grain coarsening. The extent of Austenite coarsening in the HAZ is closely related to the type and volume fraction of each microalloy precipitate.
Among the three steels, the Ti-containing HAZ exhibited the smallest extent of grain growth due to the sufficient amount of stable Ti-rich precipitates. Microalloy Addition also markedly influenced the subsequent phase transformation in the HAZ. The formation of intragranular acicular ferrite was promoted by Ti-rich precipitate, acting as favourable nucleation sites of ferrite. This structure enhanced the HAZ toughness owing to fine, high-angle boundaries of ferrite plates. The synergistic effect of Nb and Mo elements was beneficial to improve the HAZ toughness at fast cooling rates by promoting fine lower bainite formation. At high heat input, large upper bainite was formed which caused reduced toughness.
The final set of experimental work was concentrated on understanding the HAZ softening mechanisms that influenced variations in the tensile properties of the welded joints. The tensile failure in the softened HAZ or base material depended on the welding parameters and the type of steel being joined. In Ti-containing steel, increased heat Input extended the softened zone width, which caused a significant decrease in hardness and then resulted in failure in this area. Therefore, limited heat Input was used to shift failure position to base material. But this was not observed in the other two steels.
Hence, small differences in microalloy addition exhibited large variation in tensile properties. Among the three steels, Ti-containing welds were found to have the most pronounced softening, followed by Ti+V-containing welds and finally Nb-containing welds. This varied softening phenomenon was related to two significant processes supported by the results of additional dilatometry simulation: phase transformation and tempering behaviour. In the Ti-containing steel, the phase Transformation product ferrite was large-sized, as a consequence of initial large austenite grains. This led to the decreased corresponding hardness of the Ti-containing steel. Furthermore, lower tempering resistance in Ti-containing steel as compared to Nb-containing steel, resulted in additional softening effect in the softened HAZ. Therefore, steel alloy identification and heat Input during welding were critical, proven by the experimentation within the same S690QL steel grade.
This work emphasised the influence of microalloy elements on weld microstructure and mechanical properties in welded joints. Knowledge of this delicate balance between steel alloy design and appropriate welding parameters is critical for the end product. Thus, this work provides specific recommendations and results to ensure proper welding practice and steel design of microalloyed high-strength steels.
A common method for nanoparticle separation, which was introduced in 1976 by Giddings, represents asymmetrical field-flow fractionation (AF4). It is a flow based separation method, which can be theoretically used to separate particles range from 1 nm to 50 µm. However, when the particles are smaller than 10 nm, separation with AF4 will become difficult to perform. Because in this case strong separation force, which induces aggregation of particles, should be applied. This will decrease recoveries of analytes and limit its application in accurate quantitative analysis. Capillary electrophoresis (CE) is another well-developed separation technique, in which samples will be separated in relation to their electrophoretic mobility. In recent years, CE has been used to separate different kinds of nanoparticles like, gold colloids or CdSe Quantum dots. However, till now only separation of particles smaller than 50 nm was reported. Because large size distribution of bigger particles will result in strong peak broadening and long separation time.
A two-dimensional coupling of AF4 and CE might provide us a new separation method, which can extend the separation ranges of both methods and be a way to characterise particles with large size distributions.
The interest in porous anodic aluminum oxide (AAO) has been rapidly growing due to its numerous applications in separation, catalysis, energy generation and storage, electronics, and sensors. From the scientific point of view, AAO is a topical interest in soft matter fields. Spatial confinement of soft matter in nanoporous media influences its structure, thermodynamics, and mobility. Embedding polymers and liquid crystals into nanopores of AAO results in a 2D nanoconfinement of these materials. This confinement affects their properties, compared to the bulk, such as phase transition temperatures and enthalpies, molecular mobility, and architecture of the crystallization. On the other hand, discotic liquid crystals (DLCs) are a promising class of soft matter for electronic applications. This is due to their ability to organize and stack themselves into columns in a hexagonal columnar mesophase, a mesophase in between the plastic crystalline and isotropic phase, driven by the overlap of the π orbitals of their aromatic core. This leads to a high charge-carrier mobility along the column axis. Further, these columns could then be considered as “molecular nanowires”. In this study, 2,3,6,7,10,11 hexakis[hexyloxy] triphenylene (HAT6), a triphenylene based DLC, was confined into nanoporous AAO membranes. The structure, dynamics and the phase behavior of the confined HAT6 were investigated by broadband dielectric spectroscopy (BDS) and differential scanning calorimetry (DSC). HAT6 was embedded into nanoporous AAO membranes by melt infiltration in the isotropic phase under argon atmosphere. The membranes have parallel aligned cylindrical nanopores, with pore diameter of 10, 20, 25, 40, 80, 120 and 180 nm. The filling degree for each sample was checked by thermogravimetric analysis (TGA) in order to ensure complete filling. Bulk HAT6 forms a hexagonal columnar phase; in between the isotropic phase above 371 K and the plastic crystalline phase below 340 K. Unlike the bulk, the confined HAT6 split the plastic crystalline-to-hexagonal columnar phase transition in two, which might be interpret as two different phase structures; close to the wall and at the pore center. Moreover, the isotropic-to-columnar transition of the confined HAT6 shifted, with decreasing pore diameter, to lower temperatures. Furthermore, pore surfaces of a series of membranes were chemically modified, resulting in a more hydrophobic pore surface than the unmodified ones. HAT6 was embedded into the modified membranes by the same aforementioned preparation. The influence of the changed host-guest-interaction, on the structure, dynamics, and the phase behavior of HAT6 confined in the modified membranes, was also investigated by BDS and DSC.
Discotic liquid crystals (DLCs) are a promising class of soft matter for electronic applications. This is due to their ability to organize and stack themselves into columns in a hexagonal columnar mesophase, driven by the overlapping of the π orbitals of their aromatic core. This leads to a high charge-carrier mobility along the column axis. Previous studies on DLCs showed that their properties, such as phase transition temperatures and enthalpies, are susceptible to nanoconfinement. In this study, 2,3,6,7,10,11 hexakis[hexyloxy] triphenylene (HAT6), a triphenylene based DLC, was confined into parallel aligned cylindrical nanopores of anodic aluminum oxide (AAO) membranes by melt infiltration in the isotropic phase under an argon atmosphere. Furthermore, the pore surfaces of a series of membranes were chemically modified, resulting in a more hydrophobic pore surface than the unmodified ones. The structure, dynamics, and the phase behavior of HAT6 confined into modified and unmodfied nanopores of AAO were investigated by broadband dielectric spectroscopy and differential scanning calorimetry. Results will be discussed in detail.
Discotic liquid crystals (DLCs) are a promising class of soft matter for electronic applications. This is due to their ability to organize and stack themselves into columns in a hexagonal columnar mesophase, a mesophase in between the plastic crystalline and isotropic phase, driven by the overlap of the π orbitals of their aromatic core. This leads to a high charge-carrier mobility along the column axis. Further, these columns could then be considered as “molecular nanowires”.
Spatial confinement of soft matter in nanoporous media influences its structure, thermodynamic properties, and mobility. Embedding liquid crystals and polymers into nanopores of anodic aluminum oxide (AAO) results in a 2D nanoconfinement of these materials. This confinement affects their properties, compared to the bulk, such as phase transition temperatures and enthalpies, molecular mobility, and architecture of the crystallization.
In this study, 2,3,6,7,10,11 hexakis[hexyloxy] triphenylene (HAT6), a triphenylene-based DLC, was confined into nanoporous AAO membranes. The structure, dynamics and the phase behavior of the confined HAT6 were investigated by broadband dielectric spectroscopy (BDS) and differential scanning calorimetry (DSC). HAT6 was embedded into nanoporous AAO membranes by melt infiltration in the isotropic phase under argon atmosphere. The membranes have parallel aligned cylindrical nanopores, with different pore diameters in the range of 10-180 nm. Bulk HAT6 forms a hexagonal columnar phase; in between the isotropic phase above 371 K and the plastic crystalline phase below 340 K. Unlike the bulk, the confined HAT6 split the phase transitions in two or more, which might be interpret as different phase structures; close to the wall and at the pore center. Moreover, the phase transitions of the confined HAT6 shifted, with decreasing pore diameter, to lower temperatures. The dependencies of the phase transition temperatures on the pore size was well-described by the Landau-de Gennes model. Furthermore, pore surfaces of a series of membranes were chemically modified, resulting in a more hydrophobic pore surface than the unmodified ones. HAT6 was embedded into the modified membranes by the same aforementioned preparation. The influence of the changed host-guest-interaction, on the structure, dynamics, and the phase behavior of HAT6 confined in the modified membranes, was also investigated by BDS and DSC.
In this study, the molecular dynamics of two linear-shaped tetramethylated guanidinium triflates ionic liquid crystals were investigated by a combination of Broadband Dielectric Spectroscopy (BDS) and Specific Heat Spectroscopy (SHS). Three processes were detected by BDS; at low temperature γ-process, at higher temperatures α-process and at even higher temperatures conductivity. The γ-process indicates localized fluctuations, and the α-process designates cooperative fluctuations. Slightly different restrictions were found for conductivity processes of LC536 and LC537 due to the slightly different lengths of alky chains. Furthermore, the cooperative dynamics were also probed by SHS. The cooperative dynamics probed by the different techniques (BDS and SHS) compared, and assigned to the different restrictions on the cooperativity due to the difference in the sensitivity of the techniques.
Trends in fluorometry and fluorescence imaging are increasing applications of molecular and nanoscale reporters with emission > 800 nm and recently also > 1000 nm for bioanalysis, medical diagnostics, bioimaging, and safety barcodes. Mandatory for the comparison of different emitter classes and the rational design of the next generation of reporters for the short wavelength infrared (SWIR) region are reliable and quantitative photoluminescence measurements in this challenging wavelength region. This is of special relevance for nanocrystalline emitters like semiconductor quantum dots and rods as well as lanthanide-based upconversion and downconversion nanocrystals, where surface states and the accessibility of emissive states by quenchers largely control accomplishable photoluminescence quantum yields and hence, signal sizes and detection sensitivities from the reporter side. Such measurements are currently hampered by the lack of suitable methods and standards for instrument calibration and validation and quantum yield standards with emission > 800 nm and especially > 1000 nm.
In this respect, we present the design of integrating sphere setups for absolute and excitation power density-dependent measurements of emission spectra and photoluminescence quantum yields in the wavelength region of 650 to 1650 nm including calibration strategies and first candidates for potential fluorescence standards. Subsequently, selected examples for spectroscopic studies of different types of nanocrystals are presented including the upconversion and downconversion emission of differently sized and surface functionalized lanthanide-doped nanoparticles