In-operando FTIR study of ligand-linked Pt nanoparticle networks employed as catalysts in hydrogen gas micro sensors.

Microporous networks of Pt nanoparticles (NP) interlinked by aromatic diamines have recently shown prospects of application as hydrogen combustion catalysts in H2 gas microsensors. In particular with respect to long-term sensor performance, they outperformed plain Pt NP as catalysts. In this paper, electron microscopy and Fourier transform infrared (FTIR) spectroscopy data on the stability of p-phenylene diamine (PDA) and of the PDA-linked Pt NP network structure during catalyst activation and long-term sensor operation at elevated temperature (up to 120-180 °C) will be presented. For the first time, all data were collected directly from microsensor catalysts, and FTIR was performed in operando, i.e., during activation and sensor operation. While the data confirm high long-term catalyst activity far superior to that of plain Pt NP over 5 days of testing, they reveal that PDA fully decomposed during long-term sensor operation and that the network of discrete Pt nanoparticles changed to a sponge-like Pt nanostructure already during catalyst activation. These findings are at variance with previous work which assumed that stability of the PDA-linked Pt NP network is prerequisite for catalyst stability and performance.

Domain-Selective BET Ligands Yield Next-Generation Synthetic Genome Readers/Regulators with Nonidentical Cellular Functions.

SynTEF1, a prototype synthetic genome reader/regulator (SynGR), was designed to target GAA triplet repeats and restore the expression of frataxin (FXN) in Friedreich's ataxia patients. It achieves this complex task by recruiting BRD4, via a pan-BET ligand (JQ1), to the GAA repeats by using a sequence-selective DNA-binding polyamide. When bound to specific genomic loci in this way, JQ1 functions as a chemical prosthetic for acetyl-lysine residues that are natural targets of the two tandem bromodomains (BD1 and BD2) in bromo- and extra-terminal domain (BET) proteins. As next-generation BET ligands were disclosed, we tested a select set with improved physicochemical, pharmacological, and bromodomain-selective properties as substitutes for JQ1 in the SynGR design. Here, we report two unexpected findings: (1) SynGRs bearing pan-BET or BD2-selective ligands license transcription at the FXN locus, whereas those bearing BD1-selective ligands do not, and (2) rather than being neutral or inhibitory, an untethered BD1-selective ligand (GSK778) substantively enhances the activity of all active SynGRs. The failure of BD1-selective SynGRs to recruit BRD4/BET proteins suggests that rather than functioning as "epigenetic/chromatin mimics," active SynGRs mimic the functions of natural transcription factors in engaging BET proteins through BD2 binding. Moreover, the enhanced activity of SynGRs upon cotreatment with the BD1-selective ligand suggests that natural transcription factors compete for a limited pool of nonchromatin-bound BET proteins, and blocking BD1 directs pan-BET ligands to more effectively engage BD2. Taken together, SynGRs as chemical probes provide unique insights into the molecular recognition principles utilized by natural factors to precisely regulate gene expression, and they guide the design of more sophisticated synthetic gene regulators with greater therapeutic potential.

Unidirectional Electron-Tunnelling Flexible PDMS Strain Sensor with Aligned Carbon Nanotubes.

High-aspect-ratio carbon nanotubes can be directly mixed into polymers to create piezoresistive polymers. Reducing the cross-sensitivity and creating unidirectional sensitive sensors can be achieved by aligning the nanotubes before they are cured in the polymer layer. This research presents and characterises this alignment of carbon nanotubes inside polydimethylsiloxane and gives the corresponding strain sensor results. The influence on the alignment method, as well as the field strength, frequency and time is shown. An analytical model is created to investigate the sensor's behaviour and determine the effect of electron-tunnelling in the sensor. A numerical model gives insight into the necessary applied field strength, frequency and time to facilitate alignment in viscous liquids. The experimental data show a two-phase piezoresistive response; first, a linear strain response, after which the more dominant electron-tunnelling piezoresistive phase starts with high gauge factors up to k ≈ 4500 in the preferential direction, depending on the carbon nanotube concentration. Gauge factors in the orthogonal direction remain low (k ≈ 22). Finally, the dynamic stability of the sensors is proven by exposing the sensors to a cyclic strain. Small initial drifts are observed but appear to stabilise after several cycles.

Analysis of the Lifetime of Neural Implants Using In Vitro Test Structures.

The aim of this work was to measure the lifetime of neural implant test samples at two different temperatures, using a method that allows the precise measurement of the sample lifetime, further analysis with the use of Weibull statistics, and examination of the applicability of the Van't Hoff rule. The correct estimation of the lifetime of neural implants is important to avoid preliminary failures, when used in humans. The novelty lies in the precise data due to the measurement approach, the application of the Weibull statistics to neural test samples, and the examination of the Van't Hoff rule's applicability to the longevity of polyimide-based neural implant samples. Several samples that consisted of interdigitated gold strands, encapsulated in polyimide were soaked in ringer solution. One batch was soaked at a temperature of 37 °C, and another was soaked at a temperature of 57 °C. Voltage was applied and measured to identify the occurrence of failures. The long-term experiment was stopped after 458 days for the samples at 37 °C and 423 days for the samples at 57 °C, with several samples still being intact at both temperature levels. The time to failure was measured and used to identify the Weibull parameters that would describe the behavior of the samples. The median lifetime of the samples changed from 363 days at 37 °C to 138 days at 57 °C. The scale and shape factor changed from 396 and 3.7 at 37 °C to 138 and 2 at 57 °C, respectively. The measured mean, median times, and Weibull scale factors were lower than expected from the Van't Hoff rule. The use of the Van't hoff rule with 2ΔT/10°C for accelerated lifetime tests would lead to an estimation of longer lifetimes than realistic. A reaction rate constant around 1.47 appears more appropriate. While a fourfold difference in lifetime would be expected, only a 2.65-fold difference in the median lifetime and a roughly 2.2-fold difference in the mean and Weibull scale factor were observed. The shift of the Weibull shape parameter from 3.7 at 37 °C to 2 at 57 °C with rising temperatures was observed, indicating differences in failure reasons and stronger aging at lower temperatures. The used method is simple to apply and interpret and allows for a precise anticipation of sample lifetimes.

Wireless, Material-Integrated Sensors for Strain and Temperature Measurement in Glass Fibre Reinforced Composites.

Fiber reinforced plastics (FRP) offer huge potentials for energy efficient applications. Special care must be taken during both FRP fabrication and usage to ensure intended material properties and behavior. This paper presents a novel approach for the monitoring of the strain and temperature of glass fibre reinforced polymer (GFRP) materials in the context of both production process monitoring and structural health monitoring (SHM) applications. The sensor is designed to be integrated into GFRPs during the production process, and the sensor concept includes possibilities of automated placement during textile layup. To minimize sensor impact on GFRP integrity and to simplify vacuum setup and part handling, the sensor operates without the need for either wires or a battery. In the first sections of this work, sensor concept, design and prototype fabrication are presented. Subsequently, it is shown how the sensors can be used for flow front monitoring and cure estimation during GFRP production by measuring local resin temperature. The resulting specimens are then characterized regarding strain measurement capabilities, mechanical influence on the host component and overall system limitations. Average strain sensor accuracy is found to be ≤0.06 mm/m, while a maximum operation temperature of 126.9 °C and a maximum reading distance of 38 mm are measured. Based on a limited number of bending tests, no negative influence of sensor presence on breaking strength could be found. Possible applications include structural components, e.g., wind turbine blades or boat hulls.

Failure Reason of PI Test Samples of Neural Implants.

Samples that were meant to simulate the behavior of neural implants were put into Ringer's solution, and the occurring damage was assessed. The samples consist of an interdigitated gold-structure and two contact pads embedded between two Polyimide layers, resulting in free-floating structures. The two parts of the interdigitated structure have no electric contacts and are submerged in the solution during the experiment. The samples were held at temperatures of 37 and 57 ∘C in order to undergo an accelerated lifetime test and to compare the results. During the course of the experiment, a voltage was applied and measured over a resistance of 1 kOhm over time. Arduinos were used as measuring devices. As the intact samples are insulating, a sudden rise in voltage indicates a sample failure due to liquid leaking in between the two polyimide layers. Once a short-circuit occurred and a sample broke down, the samples were taken out of the vial and examined under a microscope. In virtually all cases, delamination was observable, with variation in the extent of the delaminated area. A comparison between measured voltages after failure and damage did not show a correlation between voltage and area affected by delamination. However, at a temperature of 37 ∘C, voltage remained constant most of the time after delamination, and a pin-hole lead to a lower measured voltage and strong fluctuations. Visually, no difference in damage between the 37 and the 57 ∘C samples was observed, although fluctuations of measured voltage occurred in numerous samples at a higher temperature. This difference hints at differences in the reasons for failure and thus limited applicability of accelerated lifetime tests.

Wrapper Functions for Integrating Mathematical Models into Digital Twin Event Processing.

Analog sensors often require complex mathematical models for data analysis. Digital twins (DTs) provide platforms to display sensor data in real time but still lack generic solutions regarding how mathematical models and algorithms can be integrated. Based on previous tests for monitoring and predicting banana fruit quality along the cool chain, we demonstrate how a system of multiple models can be converted into a DT. Our new approach provides a set of generic "wrapper functions", which largely simplify model integration. The wrappers connect the in- and outputs of models to the streaming platform and, thus, require only minor changes to the model software. Different scenarios for model linking structures are considered, including simultaneous processing of multiple models, sequential processing of life-cycle-specific models, and predictive models, based on data from the current and previous life cycles. The wrapper functions can be easily adapted to host models or microservices from various applications fields, to predict the future system behavior and to test what-if scenarios.

Understanding Electrical Failure of Polyimide-Based Flexible Neural Implants: The Role of Thin Film Adhesion.

The lack of long-term stability of polymeric neural interfaces remains one of the most important and less tackled issues in this research field. To address this issue, we fabricated two test structures based on interdigitated electrodes (IDEs) encapsulated with polyimide (PI). One of the test samples was pretreated with barrel oxygen plasma prior to spin coating of the second PI layer. The second test structure was pretreated using a reactive ion etching (RIE) process. The test samples were immersed in an electrolyte solution at elevated temperatures to mimic the conditions inside the human brain. The samples were then electrically and mechanically stressed to accelerate their degradation. Real-time monitoring of the electrical insulation stability was used to compare the impact of the pretreatment on the long-term stability. Barrel-plasma-activated test samples showed a mean lifetime of 1.5 days, whereas RIE pretreatment increased the mean lifetime to 24 days. Therefore, RIE-pretreated test samples exhibited 16 times longer mean stability compared to purely chemically activated test samples. Furthermore, the electrical measurements were correlated with mechanical adhesion tests. Chemically activated test samples showed significant delamination, whereas RIE pretreatment enhanced the adhesion, and no delamination could be observed. The correlation of these investigations suggests that the adhesion between different layers is higher following RIE pretreatment compared to pretreatment with chemical barrel plasma. In conclusion, the adhesion between the two PI foils seems to play a key role in the long-term stability of such devices.

MEMS Vibrometer for Structural Health Monitoring Using Guided Ultrasonic Waves.

Structural health monitoring of lightweight constructions made of composite materials can be performed using guided ultrasonic waves. If modern fiber metal laminates are used, this requires integrated sensors that can record the inner displacement oscillations caused by the propagating guided ultrasonic waves. Therefore, we developed a robust MEMS vibrometer that can be integrated while maintaining the structural and functional compliance of the laminate. This vibrometer is directly sensitive to the high-frequency displacements from structure-borne ultrasound when excited in a frequency range between its first and second eigenfrequency. The vibrometer is mostly realized by processes earlier developed for a pressure sensor but with additional femtosecond laser ablation and encapsulation. The piezoresistive transducer, made from silicon, is encapsulated between top and bottom glass lids. The eigenfrequencies are experimentally determined using an optical micro vibrometer setup. The MEMS vibrometer functionality and usability for structural health monitoring are demonstrated on a customized test rig by recording application-relevant guided ultrasonic wave packages with a central frequency of 100 kHz at a distance of 0.2 m from the exciting ultrasound transducer.

Considerations and Limits of Embedding Sensor Nodes for Structural Health Monitoring into Fiber Metal Laminates.

The objective of this article is to present the results of our investigations concerning the environmental conditions that can be expected during the embedding process into fibre metal laminates and the consequences for a sensor node for structural health monitoring. The idea behind this investigation is to determine for which manufacturing conditions the integration of sensor nodes into the material can be done and to identify limits for this. The sensor nodes consist of commercially available integrated circuits and passive components soldered onto an adhesive-less flexible printed circuit board. They are tested under conditions above their specified limits, to find out if they are still working reliably after experiencing 155 min of 180 ∘C and 7 bar of pressure. Apart from occurring temperature damage, the effect of surrounding fibres potentially pushing away the components under the amount of pressure of the manufacturing process, as well as the potential of shorts due to conductive fibers are investigated and suitable solutions to prevent this are evaluated. One experiment exceeding the typical requirements of a fiber metal laminate embedding process for structural components will be conducted at 250 ∘C for 10 h, in order to determine the limits of embedding electronic sensor nodes. This time and temperature combination is expected to cause irreversible damage to the electronic system. Results show that it is possible to integrate electronics into materials under conditions far above their specifications when precautions are taken but also that there are limits that must not be exceeded during the embedding process.

Stainless-Steel Antenna on Conductive Substrate for an SHM Sensor System with High Power Demand.

This paper presents the novel concept of structuring a planar coil antenna structured into the outermost stainless-steel layer of a fiber metal laminate (FML) and investigating its performance. Furthermore, the antenna is modified to sufficiently work on inhomogeneous conductive substrates such as carbon-fiber-reinforced polymers (CFRP) independent from their application-dependent layer configuration, since the influence on antenna performance was expected to be configuration-dependent. The effects of different stack-ups on antenna characteristics and strategies to cope with these influences are investigated. The purpose was to create a wireless self-sustained sensor node for an embedded structural health monitoring (SHM) system inside the monitored material itself. The requirements of such a system are investigated, and measurements on the amount of wireless power that can be harvested are conducted. Mechanical investigations are performed to identify the antenna shape that produces the least wound to the material, and electrical investigations are executed to prove the on-conductor optimization concept. Furthermore, a suitable process to fabricate such antennas is introduced. First measurements fulfilled the expectations: the measured antenna structure prototype could provide up to 11 mW to a sensor node inside the FML component.

Towards Long-Term Stable Polyimide-Based Flexible Electrical Insulation for Chronically Implanted Neural Electrodes.

For chronic applications of flexible neural implants, e.g., intracortical probes, the flexible substrate material has to encapsulate the electrical conductors with a long-term stability against the saline environment of the neural tissue. The biocompatible polymer polyimide is often used for this purpose. Due to its chemical inertness, the adhesion between two polyimide layers is, however, a challenge, which can lead to delamination and, finally, to short circuits. The state-of-the-art method to improve the adhesion strength is activating the polyimide surface using oxygen reactive ion etching (O2 RIE). However, the influence of the process variations (etching time, bias power) on the long-term stability is still unclear. Therefore, we establish a test method, where the aging of a gold interdigital structure embedded in two polyimide layers and immersed in saline solution is accelerated using an elevated temperature, mechanical stress and an electrical field. A continuous measurement of a leakage current is used to define the failure state. The results show that the variation of the O2 RIE plasma process has a significant effect on the long-term stability of the test samples. Comparing the two different plasma treatments 0.5 min at 25 W and 1 min at 50 W, the long-term stability could be increased from 20.9 ± 19.1 days to 44.9 ± 18.9 days. This corresponds to more than a doubled lifetime. An ideal solution for the delamination problem is still not available; however, the study shows that the fine-tuning of the fabrication processes can improve the long-term stability of chronically implanted neural electrodes.

Low-Cost and Highly Sensitive Pressure Sensor with Mold-Printed Multi-Walled Carbon Nanotubes Dispersed in Polydimethylsiloxane.

Flexible pressure sensors with piezoresistive polymer composites can be integrated into elastomers to measure pressure changes in sealings, preemptively indicating a replacement is needed before any damage or leakage occurs. Integrating small percentages of high aspect ratio multi-walled carbon nanotubes (MWCNTs) into polymers does not significantly change its mechanical properties but highly affects its electrical properties. This research shows a pressure sensor based on homogeneous dispersed MWCNTs in polydimethylsiloxane with a high sensitivity region (0.13% kPa-1, 0-200 kPa) and sensitive up to 500 kPa. A new 3D-printed mold is developed to directly deposit the conductive polymer on the electrode structures, enabling sensor thicknesses as small as 100 µm.

Synthesis and Characterization of Ligand-Linked Pt Nanoparticles: Tunable, Three-Dimensional, Porous Networks for Catalytic Hydrogen Sensing.

Porous networks of Pt nanoparticles interlinked by bifunctional organic ligands have shown high potential as catalysts in micro-machined hydrogen gas sensors. By varying the ligand among p-phenylenediamine, benzidine, 4,4''-diamino-p-terphenyl, 1,5-diaminonaphthalene, and trans-1,4-diaminocyclohexane, new variants of such networks were synthesized. Inter-particle distances within the networks, determined via transmission electron microscopy tomography, varied from 0.8 to 1.4 nm in accordance with the nominal length of the respective ligand. While stable structures with intact and coordinatively bonded diamines were formed with all ligands, aromatic diamines showed superior thermal stability. The networks exhibited mesoporous structures depending on ligand and synthesis strategy and performed well as catalysts in hydrogen gas microsensors. They demonstrate the possibility of deliberately tuning micro- and mesoporosity and thereby transport properties and steric demands by choice of the right ligand also for other applications in heterogeneous catalysis.

An Assessment of Surface Treatments for Adhesion of Polyimide Thin Films.

Polyimide films are currently of great interest for the development of flexible electronics and sensors. In order to ensure a proper integration with other materials and PI itself, some sort of surface modification is required. In this work, microwave oxygen plasma, reactive ion etching oxygen plasma, combination of KOH and HCl solutions, and polyethylenimine solution were used as surface treatments of PI films. Treatments were compared to find the best method to promote the adhesion between two polyimide films. The first selection of the treatment conditions for each method was based on changes in the contact angle with deionized water. Afterward, further qualitative (scratch test) and a quantitative adhesion assessment (peel test) were performed. Both scratch test and peel strength indicated that oxygen plasma treatment using reactive ion etching equipment is the most promising approach for promoting the adhesion between polyimide films.

An Investigation on High-Resolution Temperature Measurement in Precision Fly-Cutting.

The loads acting on a workpiece during machining processes determine the modification of the surface of the final workpiece and, thus, its functional properties. In this work, a method that uses thermocouples to measure the temperature in precision fly-cutting machining with high spatial and temporal resolution is presented. Experiments were conducted for various materials and machining parameters. We compare experimental measurement data with results from modern and advanced machining process simulation and find a good match between experimental and simulation results. Therefore, the simulation is validated by experimental data and can be used to calculate realistic internal loads of machining processes.

A Combined Thin Film/Thick Film Approach to Realize an Aluminum-Based Strain Gauge Sensor for Integration in Aluminum Castings.

There is currently a large demand for aluminum components to measure the mechanical and thermal loads to which they are subjected. With structural health monitoring, components in planes, vehicles, or bridges can monitor critical loads and potentially prevent an impending fatigue failure. Externally attached sensors need a structural model to obtain knowledge of the mechanical load at the point of interest, whereas embedded sensors can be used for direct measurement at the point of interest. To produce an embedded sensor, which is automatically encapsulated against environmental influence, the sensor must be able to withstand the boundary conditions of the host component's manufacturing process. This embedding process is particularly demanding in the case of casting. Previous work showed that silicon-based sensors have a high failure rate when embedded in cast aluminum parts and that using aluminum as a substrate is preferable under these circumstances. In the present paper, we present the fabrication process for the combination of a thick-film insulation and a thin-film strain gauge sensor, on such an aluminum substrate. The sensor is capable of withstanding high temperatures of at least 600 °C for over 20 min and a subsequent embedding in a gravity die casting process.

Design and Fabrication Challenges of a Highly Sensitive Thermoelectric-Based Hydrogen Gas Sensor.

This paper presents a highly sensitive thermoelectric sensor for catalytic combustible gas detection. The sensor contains two low-stress (+176 MPa) membranes of a combination of stoichiometric and silicon-rich silicon nitride that makes them chemically and thermally stable. The complete fabrication process with details, especially the challenges and their solutions, is discussed elaborately. In addition, a comprehensive evaluation of design criteria and a comparative analysis of different sensor designs are performed with respect to the homogeneity of the temperature field on the membrane, power consumption, and thermal sensitivity. Evaluating the respective tradeoffs, the best design is selected. The selected sensor has a linear thermal characteristic with a sensitivity of 6.54 mV/K. Additionally, the temperature profile on the membrane is quite homogeneous (20% root mean standard deviation), which is important for the stability of the catalytic layer. Most importantly, the sensor with a ligand (p-Phenylenediamine (PDA))-linked platinum nanoparticles catalyst shows exceptionally high response to hydrogen gas, i.e., 752 mV at 2% concentration.

Visual epidural field potentials possess high functional specificity in single trials.

Recordings of epidural field potentials (EFPs) allow neuronal activity to be acquired over a large region of cortical tissue with minimal invasiveness. Because electrodes are placed on top of the dura and do not enter the neuronal tissue, EFPs offer intriguing options for both clinical and basic science research. On the other hand, EFPs represent the integrated activity of larger neuronal populations and possess a higher trial-by-trial variability and a reduced signal-to-noise ratio due the additional barrier of the dura. It is thus unclear whether and to what extent EFPs have sufficient spatial selectivity to allow for conclusions about the underlying functional cortical architecture, and whether single EFP trials provide enough information on the short timescales relevant for many clinical and basic neuroscience purposes. We used the high spatial resolution of primary visual cortex to address these issues and investigated the extent to which very short EFP traces allow reliable decoding of spatial information. We briefly presented different visual objects at one of nine closely adjacent locations and recorded neuronal activity with a high-density epidural multielectrode array in three macaque monkeys. With the use of receiver operating characteristics (ROC) to identify the most informative data, machine-learning algorithms provided close-to-perfect classification rates for all 27 stimulus conditions. A binary classifier applying a simple max function on ROC-selected data further showed that single trials might be classified with 100% performance even without advanced offline classifiers. Thus, although highly variable, EFPs constitute an extremely valuable source of information and offer new perspectives for minimally invasive recording of large-scale networks.NEW & NOTEWORTHY Epidural field potential (EFP) recordings provide a minimally invasive approach to investigate large-scale neural networks, but little is known about whether they possess the required specificity for basic and clinical neuroscience. By making use of the spatial selectivity of primary visual cortex, we show that single-trial information can be decoded with close-to-perfect performance, even without using advanced classifiers and based on very few data. This labels EFPs as a highly attractive and widely usable signal.

Mechanistic Insight on the Mode of Action of Colletoic Acid.

The natural product colletoic acid (CA) is a selective inhibitor of 11ß-hydroxysteroid dehydrogenase type 1 (11ß-HSD1), which primarily converts cortisone to the active glucocorticoid (GC) cortisol. Here, CA's mode of action and its potential as a chemical tool to study intracellular GC signaling in adipogenesis are disclosed. 11ß-HSD1 biochemical studies of CA indicated that its functional groups at C-1, C-4, and C-9 were important for enzymatic activity; an X-ray crystal structure of 11ß-HSD1 bound to CA at 2.6 Å resolution revealed the nature of those interactions, namely, a close-fitting and favorable interactions between the constrained CA spirocycle and the catalytic triad of 11ß-HSD1. Structure-activity relationship studies culminated in the development of a superior CA analogue with improved target engagement. Furthermore, we demonstrate that CA selectively inhibits preadipocyte differentiation through 11ß-HSD1 inhibition, suppressing other relevant key drivers of adipogenesis (i.e., PPARγ, PGC-1α), presumably by negatively modulating the glucocorticoid signaling pathway. The combined findings provide an in-depth evaluation of the mode of action of CA and its potential as a tool compound to study adipose tissue and its implications in metabolic syndrome.