Ingenieurwissenschaften und zugeordnete Tätigkeiten
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Eingeladener Vortrag
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Experimenting on MAUS
(2019)
Everything SAXS
(2019)
The 44th Meeting of the Versailles Project on Advanced Materials and Standards (VAMAS) Steering Committee has just taken place at NIST in Boulder (CO, USA). BAM participates with significant contributions in Technical Working Areas on nanoparticle and surface chemistry characterization, but also has positioned itself to new global material challenges and trends in the developement of advanced materials and their characterization, such as thermal properties, self-healing materials, and micro- and nanoplastic.
Compatibility of polymeric materials with heating oil/biodiesel blends at different temperatures
(2019)
Materials compatibility is a major concern whenever the fuel composition is changed. The question arises of whether polymeric materials are resistant to heating oil with admixtures of 10 % biodiesel (B10) and 20 % biodiesel (B20).
The polarity of biodiesel increases its solvency and facilitates permeation and extrac-tion. Solvation, swelling and/or extraction lead to changes in the physical properties and chemical changes of polymeric materials.
The objective of this research was to determine the resistance of frequently used sealing materials such as FKM, EPDM, CR, CSM, NBR, IIR, VMQ, FVMQ, PA and PUR in up to four-year aged B10 for 84 days at 20 °C, 40 °C and 70 °C.
The polymeric materials: ACM, FKM, HNBR, PA, PE; POM, PUR and PVC were ex-posed to B20 for 84 days at 40°C and 70°C in another research project.
Mass, tensile strength, breaking elongation and Shore hardness A (D) of the test specimens were determined before and after the exposure for 84 (42) days in the heating oil blends B10 and B20.
There is not determined a threshold for the reduction in tensile properties and Shore hardness in the international standards. Therefore, a threshold of 15 % was deter-mined for the evaluation of the compatibility.
Measurements of the variations in mass, tensile properties and Shore hardness after exposure of the polymers in non-aged and aged heating oil B10 showed clearly that FKM, FVMQ and PA were the most resistant materials in B10. The elastomers CR, CSM, EPDM, IIR, NBR and VMQ were generally not resistant to B10. Damage to the materials increased with higher test temperatures and the age of B10.
FKM, POM and PVC showed high compatibility in B20 at 40°C and 70 °C. ACM, HNBR and PA were evaluated as resistant in B20 at 40 °C but not at 70°C.
In recent years superglassy polymers exhibiting intrinsic microporosity established a new perspective for a number of applications, especially for gas separation membranes as These polymers Combine extremely high permeabilities with attractive selectivities. The essential factor governing the structure Formation in the solid film or layer is either a contorted rigid Backbone (polymers of intrinsic microporosity - PIMs) or extremely bulky side groups (polynorbornenes and polytricyclonenenes).
For a deeper understanding of both types of such high-Performance polymers for gas separation membranes and their further development broadband dielectric spectroscopy (BDS) can provide a substantial contribution.
BDS addresses molecular relaxations characterizing the dynamics of the solid polymer as a major factor determining the gas transport properties but also the physical aging behavior which is an essential issue for such polymers.
BDS is applied on PIMs where fluctuations of molecular dipoles connected to the backbone can be directly monitored. Furthermore, also polynorbornenes were investigated which carry no dipole moment in their repeat unit - the high resolution of modern equipment allows for the detailed analysis also for very small dielectric losses originating from partially oxidized moieties or marginal catalyst residues.
Additionally, from interfacial polarization phenomena, such as Maxwell-Wagner-Sillars (MWS) polarization due to blocking of charge carriers at internal interfacial boundaries on a mesoscopic length scale, valuable information on the intrinsic microporosity and its changes induced by physical aging can be obtained.
Finally, also conductivity can be characterized in detail in such polymeric systems revealing contributions of interactions of aromatic moieties (π-π-stacking) or the drift motion of charge carriers. These features also determine the structure formation in the solid state.
Some critical discussion of the state of the art of uncertainty evaluationin Instrumented Indentation Testing IIT
Nowadays the Instrumented Indentation Testing (IIT), in the nano range often named as nano indention, is one of the most commonly used methods to determine the mechanical properties of materials in the micro and nano range. This method is already extensive standardized in ISO 14577 part 1-4. In the past, the application of this standard in testing praxis shows that the established values have an excellent precision.If an uncertainty is calculated, the range of values within which the true value is asserted to lie with some level of confidencewill be known. In part 1 of ISO 14577 [1] two methods for evaluation of the uncertainty in IIT are mentioned:
Method 1 for determining uncertainty considers only those uncertainties associated with the overall measurement performance of the testing machine with respect to the reference blocks.
Method 2calculates a combined uncertainty from individual contributions. These may be grouped into random and systematic uncertainties.
Both methods will be described in detail using examples from the dailyexperimental praxis. The comparabilityof both methods will be critically discussed. Finally, it will be showedhow the calculated uncertaintiescan be used for performancetests and product specifications.
Acknowledgement
This work was performed under the support of the EMPIR project 17NRM05Advancing measurement uncertainty̶ comprehensiveexamples for key international standards
References
[1] ISO 14577 part 1 (2017)
The lecture traces the origins of paper, the manufacture and the spread from China to the Middle East and Europe.
Though technological progress considerably affected each step of the manufacture of paper, the essence of the invention remains unchanged until today. The process of manufacturing handmade paper can be divided into a number of steps:
- choosing the raw material (e.g. cellulose from wood, cotton, rags)
- beating and grinding the fibres into small pieces
- producing a liquid pulp of the desired texture
- treating the pulp with various additives
- filling the pulp suspension into a paper mould
- draining the water
- pressing and drying to get the actual sheet
- various post-production treatments
We will see how the manufacturing process is reflected in the properties of the paper and its degradation. A special attention will be paid to the instrumental analysis for identification of the paper types. Also watermark play an important role in the studies of the manuscripts. A short overview will be offered at the ends of the lecture.
Inks and pigments
(2019)
The writing materials used in various cultures and epochs can be divided into two groups. The first comprises materials that write themselves, producing script by rubbing their own material off onto the writing surface. It includes charcoal, graphite, chalk, raddle, and metal styluses. Depending on the material and consistency, these are cut or pressed to make styluses and then used for writing.
The second group comprises all coloring liquids that are applied to the writing surface with a quill, pen, or printing block. It includes inks made from dye solutions (for example, tannin inks) and those made from pigment dispersions (for example, sepia, soot, and bister inks). The latter are sometimes also rubbed as pastes into letters incised into the writing surface, where they increase visual contrast.
Due to the variety of recipes and the natural origin of raw materials, there is a wide range of different components and impurities in writing materials.
Soluble inks (Tinten)
Soluble inks are based mainly on dyes forming a water solution. Colored inks were manufactured with different plant or insect dyes (e.g. Brazil wood, kermes). To stabilize the volatile material, the dyes were mixed with a mordant (e.g., alum).
Brown plant inks – best-known as blackthorn or Theophilus’ inks – are usually produced from the blackthorn bark and wine. In the early European Middle Ages, inks of this kind were widely used in the production of manuscripts in monasteries. Usually, they are light brown, so sometimes small amounts of iron sulfate were added, which led to what was called an “imperfect” iron gall ink. The difference between “classic” iron gall ink and such imperfect ink is therefore not clear: the distinction is not possible, especially with the naked eye.
Dispersion inks (Tuschen)
According to its generic recipe, one of the oldest black writing materials is produced by mixing soot with a binder dissolved in a small amount of water. Thus, along with soot, binders such as gum arabic (ancient Egypt) or animal glue (China) are among the main components of soot inks. From Pliny’s detailed account of the manufacture of various soot-based inks, we learn that, despite its seeming simplicity, producing pure soot of high quality was not an easy task in Antiquity. Therefore, we expect to find various detectable additives that might be indicative of the time and place of production. One such carbon ink requires the addition of copper sulfate . The experimental discovery of this ink in 1990 led to a misleading expression “metal ink” that is sometimes found in the literature.
Colored dispersion inks based on pigments such as orpiment, cinnabar, or azurite have been known since Antiquity. Natural or artificially produced minerals are finely ground and dispersed in a binding medium. As in soot inks, water-soluble binders such as gum arabic or egg white were used.
Iron gall ink (Eisengallustinten)
Iron gall inks are a borderline case between these two groups. They are produced from four basic ingredients: galls, vitriol as the main source of iron, gum arabic as a binding media, and an aqueous medium such as wine, beer, or vinegar. By mixing gallic acid with iron sulfate, a water-soluble ferrous gallate complex is formed; this product belongs to the type “soluble inks”. Due to its solubility, the ink penetrates the writing support’s surface, making it difficult to erase. Exposure to oxygen leads to the formation of insoluble black ferric gallate pigment, i.e., “dispersion ink”.
Natural vitriol consists of a varying mixture of metal sulfates. Since for ink making it was obtained from different mines and by various techniques, inks contain many other metals, like copper, aluminum, zinc, and manganese, in addition to the iron sulfate. These metals do not contribute to color formation in the ink solution, but possibly change the chemical properties of the inks.
Parchment
(2019)
This lecture will present history of parchment based on written sources and chemical examination of antique, medieval and modern parchment.
Our studies of the Dead Sea Scrolls writing surfaces show that they can be divided roughly into three groups: leather, parchments of a light tint, and those of various shades of brown. The latter ones are invariably tanned, whereas the middle group is characterized by the presence of various inorganic salts. Some of the pale parchments, among them the Temple Scroll (11Q19), are remarkably similar to medieval European parchment. Therefore we have formulated the working theory that in the Judaea of the Hellenistic period two different parchment-making traditions existed side by side: an ‘eastern’ one (represented by the tanned parchments of Qumran, closely resembling Aramaic documents from the fifth century BC, and a ‘western’ one (represented by the untanned/lightly tanned ones similar to early Christian Greek parchments).
This division has found support during our studies of the Geniza fragments, in which Babylonian and Palestinian traditions seem to follow the “eastern” and “western” technologies, respectively.
Chemical effects during the formation of femtosecond laser-induced periodic surface structures
(2019)
The processing of laser-induced periodic surface structures (LIPSS, ripples) on metals and semiconductors in ambient air is usually accompanied by superficial oxidation effects – a fact that is widely neglected in the current literature. In this contribution, chemical, structural, and mechanical alterations in the formation of femtosecond LIPSS are characterized by a variety of surface analytical techniques, including energy dispersive X-ray analyses (EDX), X-ray photoelectron spectroscopy (XPS), micro Raman spectroscopy (µ-RS), and depth-profiling Auger electron microscopy (AEM). Alternative routes of electrochemical and thermal oxidation allow to qualify the relevance of superficial oxidation effects on the tribological performance in oil lubricated reciprocating sliding tribological tests (RSTT). It is revealed that the fs-laser processing of near-wavelength sized LIPSS on metals leads to the formation of a few hundreds of nanometers thick graded oxide layers, consisting mainly of amorphous oxides. Regardless of reduced hardness and limited thickness, this nanostructured surface layer efficiently prevents a direct metal-to-metal contact in the RSTT and may also act as an anchor layer for specific wear-reducing additives contained in the used engine oil.
Simulational tools are applied to investigate the physical properties of nanoparticles.
For the description of radioactive gold nanoparticles, particles scattering simulations are performed with the Geant4 monte carlo simulation toolkit.
The temperature dependent behaviour of the magnetization dynamics of different magnetic nanoparticles are simulated with the object oriented micormagnetic framework (OOMMF).
Mechanochemistry is increasingly used for synthesizing soft matter materials including metal organic compounds and cocrystals. The ever-increasing interest in this method is contrasted by a limited mechanistic understanding of the mechanochemical reactivity and selectivity. Time-resolved in situ investigations of milling reactions provide direct insights in the underlying mechanisms. We introduced a setup enabling in situ investigation of mechanochemical reactions using synchrotron XRD combined with Raman spectroscopy. The specific combination allows to study milling processes comprehensively on the level of the molecular and crystalline structure and thus obtaining reliable data for mechanistic studies. We discuss our recent results investigating the formation of (polymorphic) cocrystals. First investigations of a mechanochemical synthesis under controlled temperature which allow determining the activation barrier are presented.6 Furthermore, X-ray diffraction and in situ Raman spectroscopy coupled with thermography revealed a low temperature increase during milling reactions due to the mechanical impact and clear temperature increases as a result of the reaction heat. Our results indicate that in situ investigation of milling reactions offer a new approach to tune and optimize mechanochemically synthesized compounds.
The project ProMoAM is presented. The goal of the project is to evaluate which NDT techniques or combination of techniques is suited for in-situ quality assurance in additive manufacturing of metals. To this end, also 3d-data fusion and visualization techniques are applied. Additional ex-situ NDT-techniques are used as references for defect detection and quantification. Feasability studies for NDT-techniques that are presently not applicable for in-situ use are performed as well.
The presentation gives a brief overview of the whole project and the different involved NDT-techniques.
At high temperatures and in harsh environments ceramic springs are often superior to metallic springs and allow for innovative solutions. A recently proposed application involves ceramic springs with metallized surfaces as capacitive force sensor. A strictly linear stress-strain characteristic of the spring is a precondition for such a sensor.
Helical ceramic springs with rectangular cross-section have been produced from sintered hollow cylinders. Alumina, ATZ, Y-TZP, and Ce-TZP springs with identical dimensions were characterized and compared regarding deformation behavior.
Spring deformation was investigated under various load scenarios.
Dynamic compression was performed with deformation speeds from 0.3 to 30 mm/min. Spring constants of alumina springs are strain rate independent. By contrast, Y-TZP spring constant increases by approximately 3 % within the experimental framework.
A high-precision test facility was developed to characterize spring displacement in nm range under static tensile load over long periods of time. Spring elongation with asymptotic course was observed for zirconia containing materials at room temperature. This effect is particularly strong in the case of Y-TZP. Up to 0.3 % time-dependent elongation was measured after 24 h under constant load. Deformation is completely reversible after unloading. Alumina springs do not show any time-dependent deformation under identical test conditions.
Contrary to alumina springs, a non-linear stress-strain behavior of TZP springs at room temperature was proved in both test series. It is supposed, that pseudo-elasticity caused by stress-induced phase transformation from tetragonal to monoclinic is responsible for this special behavior of TZP springs.