Pixelwise high-temperature calibration for in-situ temperature measuring in powder bed fusion of metal with laser beam.

High-temperature calibration methods in additive manufacturing involve the use of advanced techniques to accurately measure and control the temperature of the build material during the additive manufacturing process. Infrared cameras, blackbody radiation sources and non-linear optimization algorithms are used to correlate the temperature of the material with its emitted thermal radiation. This is essential for ensuring the quality and repeatability of the final product. This paper presents the calibration procedure of an imaging system for in-situ measurement of absolute temperatures and temperature gradients during powder bed fusion of metal with laser beam (PBF-LB/M) in the temperature range of 500 K-1500 K. It describes the design of the optical setup to meet specific requirements in this application area as well as the procedure for accounting the various factors influencing the temperature measurement. These include camera-specific effects such as varying spectral sensitivities of the individual pixels of the sensor as well as influences of the exposure time and the exposed sensor area. Furthermore, influences caused by the complex optical path, such as inhomogeneous transmission properties of the galvanometer scanner as well as angle-dependent transmission properties of the f-theta lens were considered. A two-step fitting algorithm based on Planck's law of radiation was applied to best represent the correlation. With the presented procedure the calibrated thermography system provides the ability to measure absolute temperatures under real process conditions with high accuracy.

Investigating bacteriophages as a novel multiple-hurdle measure against Campylobacter: field trials in commercial broiler plants.

Campylobacter mitigation along the food production chain is considered effective for minimizing the public health burden of human campylobacteriosis. This study is the first combining different measures in a multiple-hurdle approach, using drinking water additives and feed additives in single and combined application schemes in commercial broiler plants. Broiler chickens in the study groups were naturally contaminated with Campylobacter. Application of an organic acid blend via drinking water, consisting of sodium propionate, potassium sorbate, and sodium diacetate, resulted in significant reductions of up to 4.9 log10 CFU/mL in fecal samples and in cecal samples at slaughter. The application of a phage mixture, consisting of Fletchervirus phage NCTC 12673 and Firehammervirus phage vB_CcM-LmqsCPL1/1, resulted in reductions of up to 1.1 log10 CFU/mL in fecal samples 1 day after dosing. The sole administration of curcumin via feed resulted in small and inconsistent reductions. In the group receiving a combination of all tested measures, reductions of up to 1.1 log10 CFU/mL were observed. Based on the results of our field trials, it was shown that both the sole application and the combined application of mitigation measures in primary production can reduce the Campylobacter load in broiler chickens, while no synergism could be observed.

Process Monitoring Using Synchronized Path Infrared Thermography in PBF-LB/M.

Additive manufacturing processes, particularly Laser-Based Powder Bed Fusion of Metals (PBF-LB/M), enable the development of new application possibilities due to their manufacturing-specific freedom of design. These new fields of application require a high degree of component quality, especially in safety-relevant areas. This is currently ensured primarily via a considerable amount of downstream quality control. Suitable process monitoring systems promise to reduce this effort drastically. This paper introduces a novel monitoring method in order to gain process-specific thermal information during the manufacturing process. The Synchronized Path Infrared Thermography (SPIT) method is based on two synchronized galvanometer scanners allowing high-speed and high-resolution observations of the melt pool in the SWIR range. One scanner is used to steer the laser over the building platform, while the second scanner guides the field of view of an IR camera. With this setup, the melting process is observed at different laser powers, scan speeds and at different locations with respect to the laser position, in order to demonstrate the positioning accuracy of the system and to initially gain thermal process data of the melt pool and the heat-affected zone. Therefore, the SPIT system shows a speed independent overall accuracy of ±2 Pixel within the evaluated range. The system further allows detailed thermal observation of the melt pool and the surrounding heat-affected zone.

Development and Evaluation of an Improved Apparatus for Measuring the Emissivity at High Temperatures.

An improved apparatus for measuring the spectral directional emissivity in the wavelength range between 1 µm and 20 µm at temperatures up to 2400 K is presented in this paper. As a heating unit an inductor is used to warm up the specimen, as well as the blackbody reference to the specified temperatures. The heating unit is placed in a double-walled vacuum vessel. A defined temperature, as well as a homogenous temperature distribution of the whole surrounding is ensured by a heat transfer fluid flowing through the gap of the double-walled vessel. Additionally, the surrounding is coated with a high-emitting paint and serves as blackbody-like surrounding to ensure defined boundary conditions. For measuring the spectral directional emissivity at different emission angles, a movable mirror is installed in front of the specimen, which can be adjusted by a rotatable arrangement guiding the emitted radiation into the attached FTIR-spectrometer. The setup of the emissivity measurement apparatus (EMMA) and the measurement procedure are introduced, and the derived measurement results are presented. For evaluating the apparatus, measurements were performed on different materials. The determined emissivities agree well with values published in literature within the derived relative uncertainties below 4% for most wavelengths.

Opto-Thermal Investigation of Additively Manufactured Steel Samples as a Function of the Hatch Distance.

Nowadays, additive manufacturing processes are becoming more and more appealing due to their production-oriented design guidelines, especially with regard to topology optimisation and minimal downstream production depth in contrast to conventional technologies. However, a scientific path in the areas of quality assurance, material and microstructural properties, intrinsic thermal permeability and dependent stress parameters inhibits enthusiasm for the potential degrees of freedom of the direct metal laser melting process (DMLS). Especially in quality assurance, post-processing destructive measuring methods are still predominantly necessary in order to evaluate the components adequately. The overall objective of these investigations is to gain process knowledge make reliable in situ statements about component quality and material properties based on the process parameters used and emission values measured. The knowledge will then be used to develop non-destructive tools for the quality management of additively manufactured components. To assess the effectiveness of the research design in relation to the objectives for further investigations, this pre-study evaluates the dependencies between the process parameters, process emission during manufacturing and resulting thermal diffusivity and the relative density of samples fabricated by DMLS. Therefore, the approach deals with additively built metal samples made on an EOS M290 apparatus with varying hatch distances while simultaneously detecting the process emission. Afterwards, the relative density of the samples is determined optically, and thermal diffusivity is measured using the laser flash method. As a result of this pre-study, all interactions of the within factors are presented. The process variable hatch distance indicates a strong influence on the resulting material properties, as an increase in the hatch distance from 0.11 mm to 1 mm leads to a drop in relative density of 57.4%. The associated thermal diffusivity also reveals a sharp decrease from 5.3 mm2/s to 1.3 mm2/s with growing hatch distances. The variability of the material properties can also be observed in the measured process emissions. However, as various factors overlap in the thermal radiation signal, no clear assignment is possible within the scope of this work.

Influence of Different Instrument Carrying Systems on the Kinematics of the Spine of Saxophonists.

AIMS: Back strain is a common musculoskeletal complaint affecting musicians, which may be related to unsuitable playing positions causing fatigue and muscle tension. In this study, three saxophone-carrying systems (neck-strap, shoulder-strap, and Saxholder) were examined for their effects on spinal column kinematics. METHODS: The influence of saxophone-carrying systems was investigated in 14 physically healthy alto saxophonists using ultrasound topometry. Additional tests were performed on 1 subject to examine the influence of the different weights of alto, tenor, and baritone saxophones with the three different carrying systems. RESULTS: The clearest difference between two systems (shoulder-strap vs Saxholder) was found in the angle at which the player's head bows forward while playing (3.35°; 95% CI 0.44, 6.26; p=0.0272). The use of the Saxholder resulted in a physiologically favorable axial position of the head. The head posture to ankle distance showed that the shoulder-strap and Saxholder, compared to the neck-strap, allowed a sagittal straightening and therefore advantageous axially balanced body position, although the differences were not statistically significant. The Saxholder also enabled a stabilization in the frontal section of the shoulders. In additional tests on 1 subject, the coefficient of variation showed that the instruments' weights had a larger influence on the physiologically favorable balanced body position than the different carrying systems. CONCLUSION: This pilot study was able to show that the technique of sonometric examination (Zebris) is an effective way to investigate the influence of instrument-carrying systems on the kinematics of the spine. The Saxholder may be physiologically advantageous, but further research with a larger sample is needed to verify the findings.

Preparation of multifunctional polysaccharide microcontainers for lipophilic bioactive agents.

Chitosan/xanthan gum microcontainers with a core-shell structure formed due to chemical interactions between polysaccharide chains induced by ultrasonication are presented. Containers were prepared by sonication of water-immiscible (oil-like) liquids in the solution of polysaccharides. One-step fabrication of the container permanent shell is possible, because of the contribution of ultrasonically caused formation of hydrogen bonds and amide linkages. We synthesized containers in a wide size range from 350 nm to 7500 nm, varying in oil/water ratio. The microcontainers were modified with oppositely charged polyelectrolytes and microparticles, which could be used to impart the specified properties to the system. The biocide 4,5-dichloro-2-n-octyl-4-isothiazoline-3-one (DCOIT) was loaded into the proposed containers by utilizing its solution as an oil phase. The following incorporation of the DCOIT containers into the polymer coating demonstrated more sustained antimicrobial activity (∼30%) of the biocide in the encapsulated state, compared to its non-encapsulated form.

Stabile, thermoresponsive colloidal clusters: an unusual morphology of polymer dispersions.

A new class of colloidal polymeric particles consisting of polystyrene spheres grown in a poly(N-isopropyl acrylamide) precursor scaffold is synthesized via redox-initiated heterophase polymerization. The morphology and thermoresponsiveness of these assemblies is proven by electron microscopy investigations and temperature-dependent measurements of the change of both the speed of sound travelling through the dispersion and the hydrodynamic particle size. Electron microscopy (EM) micrographs (transmission and scanning EM as well cryo-scanning EM) prove the existence of colloidal clusters when the freeze-dried copolymer is redispersed in pure water. The clusters have a size of several micrometers, contain about 800 polystyrene particles with diameter below 100 nm, and show a highly reproducible thermoresponsive behavior with a lower critical solution temperature corresponding to that of pure poly(N-isopropyl acrylamide).

Nanoplasmonic modification of the local morphology, shape, and wetting properties of nanoflake microparticles.

Inducing a phase transition of a self-organized object may trigger its structural transformation. Here, we demonstrate local control of the morphology and shape of self-organized microparticles with a nanoflake outer surface by nanoplasmonic heating. To increase the photothermal efficiency of the microparticles, gold nanoparticles (AuNPs) or single-walled carbon nanotubes (SWCNTs) were incorporated. AuNPs and SWCNTs, which have excellent photothermal activity, acts as photoresponsive heat converters. Because they have distinct absorption characteristics, visible or near-infrared lasers can be used to induce local heating. The photothermal effect was used to spatially confine the melting to the space within the particle and the aggregate; as a result, microparticles with various shapes and morphologies have been fabricated. Such morphological changes lead to a superhydrophobic-hydrophobic wetting transition, which was confirmed by the films constituting the microparticles. The work presented is seen useful for anisotropic particle synthesis, local wetting control, lithography, and morphological control of functional materials.

Synthesis of porous PEG microgels using CaCO3 microspheres as hard templates.

Porous poly(ethylene glycol) (PEG) microgels of both 17.6 and 8.3 µm in diameter are synthesized via hard templating with calcium carbonate (CaCO(3)) microparticles. The synthesis is performed in three steps: loading of PEG macromonomers into CaCO(3) microparticles, crosslinking via photopolymerization, and removal of the CaCO(3) template under acidic conditions. The resulting porous PEG microgels are inverse replicates of their templates as indicated by light microscopy, cryo-scanning electron microscopy (cryo-SEM), and permeability studies. Thus this process allows for the straightforward and highly reproducible synthesis of porous hydrogel particles of two different diameters and porosities that show great potential as carriers for drugs or nanomaterials.

Metabolic profiling of Arabidopsis thaliana epidermal cells.

Metabolic phenotyping at cellular resolution may be considered one of the challenges in current plant physiology. A method is described which enables the cell type-specific metabolic analysis of epidermal cell types in Arabidopsis thaliana pavement, basal, and trichome cells. To achieve the required high spatial resolution, single cell sampling using microcapillaries was combined with routine gas chromatography-time of flight-mass spectrometry (GC-TOF-MS) based metabolite profiling. The identification and relative quantification of 117 mostly primary metabolites has been demonstrated. The majority, namely 90 compounds, were accessible without analytical background correction. Analyses were performed using cell type-specific pools of 200 microsampled individual cells. Moreover, among these identified metabolites, 38 exhibited differential pool sizes in trichomes, basal or pavement cells. The application of an independent component analysis confirmed the cell type-specific metabolic phenotypes. Significant pool size changes between individual cells were detectable within several classes of metabolites, namely amino acids, fatty acids and alcohols, alkanes, lipids, N-compounds, organic acids and polyhydroxy acids, polyols, sugars, sugar conjugates and phenylpropanoids. It is demonstrated here that the combination of microsampling and GC-MS based metabolite profiling provides a method to investigate the cellular metabolism of fully differentiated plant cell types in vivo.

Synthesis of monodisperse quasi-spherical gold nanoparticles in water via silver(I)-assisted citrate reduction.

We demonstrate a simple and reproducible way to produce quasi-spherical Au nanoparticles (NPs) with a fairly narrow size distribution in water by rapidly adding a mixture solution of HAuCl(4), sodium citrate, and a trace amount of silver nitrate into boiling water. The sizes of quasi-spherical Au NPs obtained increases from 12 +/- 1 nm to 18 +/- 3, 25 +/- 3, and 36 +/- 3 nm with decrease of the citrate concentration in a fairly linear way. The present protocol can efficiently minimize the effect of citrate to buffer the pH of the reaction media and thus change the type and reactive activity of auric ions and significantly speed up the nucleation and growth rate of Au NPs. The presence of Ag(+) ions can not only suppress the secondary nucleation but also reshape the polycrystalline Au NPs into a quasi-spherical shape. In the case of synthesis of Au NPs of sizes ranging from 10 to 36 nm, our approach efficiently makes up the shortages of the classical Turkevich method with respect to the reproducibility and uniformity of the NP size and shape.

Polyelectrolyte-directed nanoparticle aggregation: systematic morphogenesis of calcium carbonate by nonclassical crystallization.

Besides the classical atom/ion/molecule based mechanism, nonclassical crystallization provides a nanoparticle-based crystallization pathway toward single crystals. However, there is a lack of experimentally established strategies for engineering a range of crystalline microstructures from common nanoparticles by nonclassical crystallization. We demonstrate that a commercial random copolymer polyelectrolyte poly(4-styrene sulfonate)-co-(maleic acid) (PSS-co-MA) considerably guides crystallization of calcium carbonate (CC) with a high versatility. The bioinspired nonclassical crystallization protocol yielded a series of calcite microstructures. Calcite single crystals obtained at low supersaturation show a pseudo-dodecahedral shape with curved faces, whereas increasing supersaturation generated calcite mesocrystals with pseudo-octahedral shapes and scalloped surfaces. Further increase of supersaturation induced the formation of polycrystalline multilayered and hollow spheres. In the initial growth stage of all these microstructures, amorphous CC nanoparticles formed as the early product. Remarkably, microparticles with minimal primitive (P)-surface were captured as the prominent intermediate indicative of liquidlike behavior. Moreover, nanogranular structures exist broadly in the as-synthesized crystals. These results demonstrate that the polyelectrolyte can effectively stabilize the amorphous CC nanoparticle precursors, impart control over the evolution from amorphous precursors via a liquid aggregate through P-surface intermediates to the final crystals, and thus allow the morphogenesis. Simple variation of calcium and polyeletrolyte concentrations enables a systematic control over the size and morphology of particles among pseudo-dodecahedra, pseudo-octahedra, multilayered spheres, and hollow spheres, which are expressed in a morphology diagram. A unifying nanoparticle aggregation formation mechanism was suggested to explain the morphogenesis by the combination of nonclassical crystallization and surface area minimization principles.

Unprecedented, low cytotoxicity of spongelike calcium phosphate/poly(ethylene imine) hydrogel composites.

Covalently crosslinked PEI hydrogels are efficient templates for calcium phosphate mineralization in SBF. In contrast to the PEI hydrogels, non-crosslinked PEI does not lead to calcium phosphate nucleation and growth in SBF. The precipitate is a mixture of brushite and hydroxyapatite. The PEI/calcium phosphate composite material exhibits a sponge like morphology and a chemical composition that is interesting for implants. Cytotoxicity tests using Dictyostelium discoideum amoebae show that both the non-mineralized and mineralized hydrogels have a very low cytotoxicity. This suggests that next generation PEI hydrogels, where also the degradation products are non-toxic, could be interesting for biomedical applications.

A subtilisin-like serine protease essential for mucilage release from Arabidopsis seed coats.

During Arabidopsis seed development large quantities of mucilage, composed of pectins, are deposited into the apoplast underneath the outer wall of the seed coat. Upon imbibition of mature seeds, the stored mucilage expands through hydration and breaks the outer cell wall that encapsulates the whole seed. Mutant seeds carrying loss-of-function alleles of AtSBT1.7 that encodes one of 56 Arabidopsis thaliana subtilisin-like serine proteases (subtilases) do not release mucilage upon hydration. Microscopic analysis of the mutant seed coat revealed no visible structural differences compared with wild-type seeds. Weakening of the outer primary wall using cation chelators triggered mucilage release from the seed coats of mutants. However, in contrast to mature wild-type seeds, the mutant's outer cell walls did not rupture at the radial walls of the seed coat epidermal cells, but instead opened at the chalazal end of the seed, and were released in one piece. In atsbt1.7, the total rhamnose and galacturonic acid contents, representing the backbone of mucilage, remained unchanged compared with wild-type seeds. Thus, extrusion and solubility, but not the initial deposition of mucilage, are affected in atsbt1.7 mutants. AtSBT1.7 is localized in the developing seed coat, indicating a role in testa development or maturation. The altered mode of rupture of the outer seed coat wall and mucilage release indicate that AtSBT1.7 triggers the accumulation, and/or activation, of cell wall modifying enzymes necessary either for the loosening of the outer primary cell wall, or to facilitate swelling of the mucilage, as indicated by elevated pectin methylesterase activity in developing atsbt1.7 mutant seeds.

Structural and analytical studies of silica accumulations in Equisetum hyemale.

Horsetail (Equisetum spp.) is known as one of the strongest accumulators of silicon among higher terrestrial plants. We use the combination of position-resolved analytical techniques, namely microtomography, energy-dispersive X-Ray elemental mapping, Raman microscopy, as well as small-angle and wide-angle scattering of X-rays, to study the type, distribution and nanostructure of silica in the internodes of Equisetum hyemale. The predominant silicification pattern is a thin continuous layer on the entire outer epidermis with the highest density in particular knob regions of the long epidermal cells. The knob tips contain up to 33 wt% silicon in the form of pure hydrated amorphous silica, while the silica content is lower in the inner part of the knobs and on the continuous layer. In contrast to the knob tips, the silica in these regions lacks silanol groups and is proposed to be in close association with polysaccharides. No mentionable amount of crystalline silica is detected by wide-angle X-ray scattering. The small-angle X-ray scattering data are consistent with the presence of colloidal, sheet-like silica agglomerates with a thickness of about 2 nm. From these results we conclude that there are at least two distinct forms of silica in E. hyemale which may have different functions. The close association of silica with cell wall polymers suggests that they may act as a polymeric template that controls the shape and size of the colloidal silica particles similar to many other biominerals and mineralised tissues. We propose that owing to its specific distribution in E. hyemale, a protective role and possibly also an important biomechanical role are among the most likely functions of silica in these plants.

Synthesis of DL-alanine hollow tubes and core-shell mesostructures.

Three double hydrophilic block copolymers were used as crystal-growth modifiers of DL-alanine to generate amorphous precursor nanoparticles that undergo subsequent mesoscopic transformation to core-shell mesostructures and hollow tubes with quadratic cross-sections. The growth sequence can be stopped at various stages so that a series of intermediates between amorphous core- and crystalline-shell particles and tubes can be obtained. Time-dependent conductivity, TEM, SEM, and environmental scanning electron microscopy (ESEM) measurements were used to obtain a better understanding of the crystallization process, and a formation mechanism for the generation of the tubes is proposed. Na2SO4, NaCl, and NaNO3 as salts differ in their influence on the crystallization behavior of alanine by changing the solubility of alanine and by decreasing the stability of the intermediate particles. Core-shell mesostructures that formed in the dissolution-recrystallization process were captured as the transformation rate was decreased by the addition of copolymers or salts. Hollow tubes with quadratic cross-sections are the final product of the transformation process.

Correct consideration of the index of refraction using blackbody radiation.

The correct consideration of the index of refraction when using blackbody radiators as standard sources for optical radiation is derived and discussed. It is shown that simply using the index of refraction of air at laboratory conditions is not sufficient. A combination of the index of refraction of the media used inside the blackbody radiator and for the optical path between blackbody and detector has to be used instead. A worst case approximation for the introduced error when neglecting these effects is presented, showing that the error is below 0.1 % for wavelengths above 200 nm. Nevertheless, for the determination of the spectral radiance for the purpose of radiation temperature measurements the correct consideration of the refractive index is mandatory. The worst case estimation reveals that the introduced error in temperature at a blackbody temperature of 3000 degrees C can be as high as 400 mk at a wavelength of 650 nm and even higher at longer wavelengths.

From ultrathin capsules to biaqueous vesicles.

The layer-by-layer (LbL) adsorption of anionic polyelectrolytes (PE) and tobramycin sulfate (TbS) multilayers on zinc oxide core particles followed by the controlled core-removal process leads to the formation of ultrathin capsules, which gradually convert to biaqueous vesicles and emulsionlike systems depending on the hydrophilicity/hydrophobicity of the PE backbone, PE/TbS ratio, and Zn2+ concentration. The unique characteristics of the PE/TbS multilayer capsules result because of the formation of PE/TbS/H2O biphasic liquid systems unlike the other LbL capsular systems that form stiff PE coacervates when mixed together in water. This paper investigates the PE/TbS ultrathin capsule to biaqueous vesicle transition and its physicochemical properties.