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At least 181 records · Page 10

A universal all-solid synthesis for high throughput production of halide perovskite

Abstract Halide perovskites show ubiquitous presences in growing fields at both fundamental and applied levels. Discovery, investigation, and application of innovative perovskites are heavily dependent on the synthetic methodology in terms of time-/yield-/effort-/energy- efficiency. Conventional wet chemistry method provides the easiness for growing thin film samples, but represents as an inefficient way for bulk crystal synthesis. To overcome these, here we report a universal solid state-based route for synthesizing high-quality perovskites, by means of simultaneously applying both electric and mechanical stress fields during the synthesis, i.e., the electrical and mechanical field-assisted sintering technique. We employ various perovskite compositions and arbitrary geometric designs for demonstration in this report, and establish such synthetic route with uniqueness of ultrahigh yield, fast processing and solvent-free nature, along with bulk products of exceptional quality approaching to single crystals. We exemplify the applications of the as-synthesized perovskites in photodetection and thermoelectric as well as other potentials to open extra chapters for future technical development.

36 MATERIALS SCIENCE↗

Procedure for developing experimental designs for accelerated tests for service-life prediction

Recommended design procedures to reduce the complete factorial design by retaining information on anticipated important interaction effects, and by generally giving up information on unconditional main effects are discussed. A hypothetical photovoltaic module used in the test design is presented. Judgments were made of the relative importance of various environmental stresses such as UV radiation, abrasion, chemical attack, temperature, mechanical stress, relative humidity and voltage. Consideration is given to a complete factorial design and its graphical representation, elimination of selected test conditions, examination and improvement of an engineering design, and parametric study. The resulting design consists of a mix of conditional main effects and conditional interactions and represents a compromise between engineering and statistical requirements.

Thomas, R. E.↗

Fabrication of Pop-up Detector Arrays on Si Wafers

High sensitivity is a basic requirement for a new generation of thermal detectors. To meet the requirement, close-packed, two-dimensional silicon detector arrays have been developed in NASA Goddard Space Flight Center. The goal of the task is to fabricate detector arrays configured with thermal detectors such as infrared bolometers and x-ray calorimeters to use in space fliGht missions. This paper focuses on the fabrication and the mechanical testing of detector arrays in a 0.2 mm pixel size, the smallest pop-up detectors being developed so far. These array structures, nicknamed "PUDS" for "Pop-Up Detectors", are fabricated on I pm thick, single-crystal, silicon membranes. Their designs have been refined so we can utilize the flexibility of thin silicon films by actually folding the silicon membranes to 90 degrees in order to obtain close-packed two-dimensional arrays. The PUD elements consist of a detector platform and two legs for mechanical support while also serving as electrical and thermal paths. Torsion bars and cantilevers connecting the detector platform to the legs provide additional flexures for strain relief. Using micro-electromechanical structure (MEMS) fabrication techniques, including photolithography, anisotropic chemical etching, reactive-ion etching, and laser dicing, we have fabricated PLTD detector arrays of fourteen designs with a variation of four parameters including cantilever length, torsion bar length and width, and leg length. Folding tests were conducted to test mechanical stress distribution for the array structures. We obtained folding yields and selected optimum design parameters to reach minimal stress levels. Computer simulation was also employed to verify mechanical behaviors of PUDs in the folding process. In addition, scanning electron microscopy was utilized to examine the flatness of detectors and the alignment of detector pixels in arrays. The fabrication of thermistors and heaters on the pop-up detectors is under way, preparing us for the next step of the experiment, the thermal test.

Li, Mary J.↗

Thermal loading effects on chalk hydromechanical behavior for nuclear waste disposal

Safe disposal of heat-generating nuclear waste depends on host rock stability under thermal, hydrological, and mechanical stresses. This study investigates the effect of thermal loading on mechanical behavior of the shallowly buried Ghareb formation chalk through triaxial and hydrostatic constant strain rate and creep tests at temperatures up to 100 ˚C and effective pressures up to 20.7 MPa. Experimental results show that thermal loading reduces the elastic moduli of chalk by 50–75%, and a transition occurs above 60 ˚C where creep rates increase rapidly. Water saturation nearly doubles the thermally induced strain compared to dry conditions and strongly decreases material rigidity. Thermal loading also leads to significant pore pressure increases under undrained conditions and leads to reductions in the apparent permeability during drained conditions. Laboratory experimental data were used to parameterize and develop a preliminary constitutive model for predicting future deformation during repository operations in the Ghareb. The strongly coupled effects – mechanical weakening, fluid pressure fluctuations, and permeability modification – demonstrate that elevated repository temperatures will have a pronounced effect on the near field Ghareb behavior during waste disposal operations. The findings indicate that the coupled interactions must be considered in predictive models and repository design to ensure long-term nuclear waste isolation and safety.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Nickel-Graphite Composite Compliant Interface and/or Hot Shoe Material

Next-generation high-temperature thermoelectric-power-generating devices will employ segmented architectures and will have to reliably withstand thermally induced mechanical stresses produced during component fabrication, device assembly, and operation. Thermoelectric materials have typically poor mechanical strength, exhibit brittle behavior, and possess a wide range of coefficient of thermal expansion (CTE) values. As a result, the direct bonding at elevated temperatures of these materials to each other to produce segmented leg components is difficult, and often results in localized microcracking at interfaces and mec hanical failure due to the stresses that arise from the CTE mismatch between the various materials. Even in the absence of full mechanical failure, degraded interfaces can lead to increased electrical and thermal resistances, which adversely impact conversion efficiency and power output. The proposed solution is the insertion of a mechanically compliant layer, with high electrical and thermal conductivity, between the low- and high-temperature segments to relieve thermomechanical stresses during device fabrication and operation. This composite material can be used as a stress-relieving layer between the thermoelectric segments and/or between a thermoelectric segment and a hot- or cold-side interconnect material. The material also can be used as a compliant hot shoe. Nickel-coated graphite powders were hot-pressed to form a nickel-graphite composite material. A freestanding thermoelectric segmented leg was fabricated by brazing the compliant pad layer between the high-temperature p- Zintl and low-temperature p-SKD TE segments using Cu-Ag braze foils. The segmented leg stack was heated in vacuum under a compressive load to achieve bonding. The novelty of the innovation is the use of composite material that re duces the thermomechanical stresses en - countered in the construction of high-efficiency, high-temperature therm - o-electric devices. The compliant pad enables the bonding of dissimilar thermoelectric materials while maintaining the desired electrical and thermal properties essential for efficient device operation. The modulus, CTE, electrical, and thermal conductances of the composite can be controlled by varying the ratio of nickel to graphite.

Firdosy, Samad A.↗

A Novel Instrument and Methodology for the In-Situ Measurement of the Stress in Thin Films

We introduce a novel methodology for the in-situ measurement of mechanical stress during thin film growth utilizing a highly sensitive non-contact variation of the classic spherometer. By exploiting the known spherical deformation of the substrate the value of the stress induced curvature is inferred by measurement of only one point on the substrate's surface-the sagittal. From the known curvature the stress can be calculated using the well-known Stoney equation. Based on this methodology, a stress sensor has been designed which is simple, highly sensitive, compact, and low cost. As a result of its compact nature, the sensor can be mounted in any orientation to accommodate a given deposition geometry without the need for extensive modification to an already existing deposition system. The technique employs the use of a double side polished substrate that offers good specular reflectivity and is isotropic in its mechanical properties, such as <111> oriented crystalline silicon or amorphous soda lime glass, for example. The measurement of the displacement of the uncoated side during deposition is performed with a high resolution (i.e. 5nm), commercially available, inexpensive, fiber optic sensor which can be used in both high vacuum and high temperature environments (i.e. 10(exp-7) Torr and 480oC, respectively). A key attribute of this instrument lies in its potential to achieve sensitivity that rivals other measurement techniques such as the micro cantilever method but, due to the comparatively larger substrate area, offers a more robust and practical alternative for subsequent measurement of additional characteristics of the film that can might be correlated to film stress. We present measurement results of nickel films deposited by magnetron sputtering which show good qualitative agreement to the know behavior of polycrystalline films previously reported by Hoffman.

Broadway, David M.↗

Experimental Identification and Simulation of Time and/or Rate Dependent Reversible and Irreversible Deformation Regions for both a Titanium and Nickel Alloy

In this paper time and/or rate dependent deformation regions are experimentally mapped out as a function of temperature. It is clearly demonstrated that the concept of a threshold stress (a stress that delineate reversible and irreversible behavior) is valid and necessary at elevated temperatures and corresponds to the classical yield stress at lower temperatures. Also the infinitely slow modulus, (Es) i.e. the elastic modulus of the material if it was loaded at an infinitely slow strain rate, and the "dynamic modulus", modulus, Ed, which represents the modulus of the material if it is loaded at an infinitely fast rate are used to delineate rate dependent from rate independent regions. As demonstrated at elevated temperatures there is a significant difference between the two modulus values, thus indicating both significant time-dependence and rate dependence. In the case of the nickel-based super alloy, ME3, this behavior is also shown to be grain size specific. Consequently, at higher temperatures viscoelastic behavior exist below k (i.e., the threshold stress) and at stresses above k the behavior is viscoplastic. Finally a multi-mechanism, stress partitioned viscoelastic model, capable of being consistently coupled to a viscoplastic model is characterized over the full temperature range investigated for Ti-6-4 and ME3.

Arnold, Steven M.↗

Chemo-Mechanical Behavior and Stability of High-Loading Cathodes in Solid-State Batteries

Solid-state batteries can offer higher energy density and improved safety compared to lithium ion batteries, which use flammable liquid electrolytes. Increasing the ratio of cathode active materials in composite cathodes enhances the energy density and reduces manufacturing costs. Changes in the ratio of cathode active materials alter the microstructure and chemo-mechanical response of a cathode during operation. Understanding the relationship between composition, microstructure, and chemo-mechanical interactions is critical for optimizing solid-state cathodes. Here, in this study, we engineered composite cathodes with varying ratios of LiNi 0.8 Co 0.1 Mn 0.1 O 2 and Li 6 PS 5 Cl to systematically investigate the role of microstructural evolution in long-term chemo-mechanical transformations. Chemo-mechanical stresses resulting from the volume changes of the cathode active materials led to degradation mechanisms, such as fracture and interfacial delamination. Active material fracture and delamination led to underutilization of active material and significant capacity decay during cycling. Coatings that suppress active material-active material interactions during cycling may aid in suppressing the generation of local stress hotspots.

36 MATERIALS SCIENCE↗

Polymers used in 4 mm PV Connectors [Slides]

Polymer cracks are not a new problem in the PV industry. However, the suddenness and severity of the cracking connector model is new and concerning. Some sites are experiencing wide-spread cracking of a specific connector model. The preliminary investigation results are (1) there are potential clearance issues with the O-ring, leading to high mechanical stress; (2) potential use of lubrication yields polymer embrittlement; and (3) clear mechanical or chemical differences between the affected model and other PPE-based models using FTIR and tensile testing could not be demonstrated.

36 MATERIALS SCIENCE↗

Evaluation of the Effect of Surface Finish on High-Cycle Fatigue for SLM-IN718

A high-cycle fatigue (HCF) knockdown factor was estimated for Inconel 718, manufactured with the selective laser melt (SLM) process. This factor is the reduction at a common fatigue life from the maximum stress in fatigue for low-stress ground (LSG) specimens to the maximum stress of those left with the original surface condition. Various vendors provided specimens. To reduce the number of degrees-of-freedom, only one heat treat condition was evaluated. Testing temperatures included room temperature, 800F, 1000F, and 1200F. The two surface conditions were compared at constant lives, where data was available. The recommended knockdown factor of the as-built surface condition (average roughness of approximately 245 micro-inches/inch) versus low-stress ground condition (roughness <= 4 micro-inches/inch) is approximately 1/3 or 33%. This is to say that for the as-built surface condition, a maximum stress of 2/3 of the stress for LSG can be expected to produce the same life in the as built surface condition. As an alternative method, the surface finish was incorporated into a new parameter with the maximum stress. The new parameter was formulated to be similar to the fracture mechanics stress intensity factor, and it was named the pseudo stress intensity factor, Kp. Using Kp, the variance seemed acceptable across all sources, and the knockdown factor was estimated over the range of data identified by Kp where data occurred. A plot of the results suggests that the knockdown factor is a function of temperature, and that for low lives the knockdown is greater than the knockdown observed above about one million cycles, where it stabilizes. One data point at room temperature was clearly different, and the sparsity of data in the higher life region reduces the value of these results. The method does appear to provide useful results, and further characterization of the method is suggested.

Lambert, Dennis M.↗

Optimized suspension culture: the rotating-wall vessel

Suspension culture remains a popular modality, which manipulates mechanical culture conditions to maintain the specialized features of cultured cells. The rotating-wall vessel is a suspension culture vessel optimized to produce laminar flow and minimize the mechanical stresses on cell aggregates in culture. This review summarizes the engineering principles, which allow optimal suspension culture conditions to be established, and the boundary conditions, which limit this process. We suggest that to minimize mechanical damage and optimize differentiation of cultured cells, suspension culture should be performed in a solid-body rotation Couette-flow, zero-headspace culture vessel such as the rotating-wall vessel. This provides fluid dynamic operating principles characterized by 1) solid body rotation about a horizontal axis, characterized by colocalization of cells and aggregates of different sedimentation rates, optimally reduced fluid shear and turbulence, and three-dimensional spatial freedom; and 2) oxygenation by diffusion. Optimization of suspension culture is achieved by applying three tradeoffs. First, terminal velocity should be minimized by choosing microcarrier beads and culture media as close in density as possible. Next, rotation in the rotating-wall vessel induces both Coriolis and centrifugal forces, directly dependent on terminal velocity and minimized as terminal velocity is minimized. Last, mass transport of nutrients to a cell in suspension culture depends on both terminal velocity and diffusion of nutrients. In the transduction of mechanical culture conditions into cellular effects, several lines of evidence support a role for multiple molecular mechanisms. These include effects of shear stress, changes in cell cycle and cell death pathways, and upstream regulation of secondary messengers such as protein kinase C. The discipline of suspension culture needs a systematic analysis of the relationship between mechanical culture conditions and biological effects, emphasizing cellular processes important for the industrial production of biological pharmaceuticals and devices.

Non-NASA Center↗

Failure Mode Identification of Insulin Drug Products – Impact of Relevant Stress Conditions on the Quality of the Drug

Fast-acting insulin drug products (DPs) are carried and administered by diabetic patients to maintain their blood glucose level throughout the day, exposing the DPs to stress conditions. Apidra, Novolog, and Humalog insulin DPs were tested under various stress conditions. Dynamic light scattering (DLS), and size exclusion chromatography (SEC) were used to monitor the stability and aggregation. Thermal stress alone did not influence the stability. However, 24 hr exposure to vigorous mechanical stress shifted the DLS size peaks of Novolog and Humalog from 5 ± 1 nm to > 50.9 ± 25.6 nm, and the SEC native protein peak areas decreased 52% for Novolog and 18.4% for Humalog. Combined stress accelerated protein aggregation more drastically. Novolog and Humalog size shifted (>75 nm) after 3 hr and the peak area decreased > 97.9% after 6 hr exposure, indicating that high temperature accelerated the aggregation triggered by agitation. Soluble aggregates were captured by DLS early on compared to SEC. Apidra was comparably stable indicating DP formulation plays a critical role in stability. Here this study provides a greater understanding of potential failure modes patients and care givers may encounter while handling insulin DPs.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Evaluation of the Effect of Surface Finish on High-Cycle Fatigue of SLM-IN718

The surface finish of parts produced by additive manufacturing processes is much rougher than the surface finish generated by machining processes, and a rougher surface can reduce the fatigue strength of a part. This paper discusses an effort to quantify that reduction of strength in high-cycle fatigue for selective laser melt (SLM) coupons. A high-cycle fatigue (HCF) knockdown factor was estimated for Inconel 718, manufactured with the SLM process. This factor is the percentage reduction from the maximum stress in fatigue for low-stress ground (LSG) specimens to the maximum stress of those left with the original surface condition at the same fatigue life. Specimens were provided by a number of vendors, free to use their "best practice"; only one heat treat condition was considered; and several test temperatures were characterized, including room temperature, 800F, 1000F, and 1200F. The 1000F data had a large variance, and was omitted from consideration in this document. A first method used linear approximations extracted from the graphs, and only where data was available for both. A recommended knockdown factor of the as-built surface condition (average roughness of approximately 245 micro-inches/inch) versus low-stress ground condition (roughness no more than 4 micro-inches/inch) was established at approximately 1/3 or 33%. This is to say that for the as-built surface condition, a maximum stress of 2/3 of the stress for LSG can be expected to produce a similar life in the as-built surface condition. In this first evaluation, the knockdown factor did not appear to be a function of temperature. A second approach, the "KP method", incorporated the surface finish measure into a new parameter termed the pseudo-stress intensity factor, Kp, which was formulated to be similar to the fracture mechanics stress intensity factor. Using Kp, the variance seemed to be reduced across all sources, and knockdown factors were estimated using Kp over the range where data occurred. A plot of the results suggests that the knockdown factor is a function of temperature, and that for low lives the knockdown might be lower than the knockdown observed above about one million cycles, where it tended to stabilize. This was not universal for all temperatures tested. The higher temperature tests are thought to be influenced by the test temperature, which perhaps continued the aging process. Further evaluation of the method is suggested.

Lambert, D. M.↗

Encapsulation Residual Stress and Ferrite Loss in Inductive Coil Assemblies

As inductive wireless charging reaches higher power levels, thermal management and mechanical durability become more critical. To address these concerns, past works have demonstrated the benefit of encapsulating coil assemblies in thermally conductive materials. However, due to the sensitivity of the MnZn ferrites commonly used in coil assemblies to mechanical stress, care must be taken to avoid creating large stresses in the ferrite that cause higher hysteresis loss. The stress formation in the encapsulant curing process is overviewed and modeled and an experiment is performed to demonstrate the effect in a small-scale coil assembly. Finally, the effect is shown in the reduced coil-coil efficiency of a first generation high power inductive power transfer prototype using a stiff epoxy compared to better performance in a second prototype using a softer thermally-conductive silicone encapsulant.

Foote, Andrew↗

Mechanical Toughening of Two-Dimensional Covalent Organic Frameworks Enabled by Graphene-Based Sandwich-Structured Nanocomposites

Low resistance to fracture in two-dimensional covalent organic frameworks (2D COFs) limits their practical applications, especially in mechanically demanding fields, such as flexible electronics and sensing devices. We address this critical limitation by fabricating a sandwich-structured nanocomposite consisting of graphene layers sandwiched between 2D COF layers (2D COFs/graphene/2D COFs) via chemical vapor deposition. Here, our sandwich-structured nanocomposites exhibit a remarkable improvement in modulus E, fracture toughness K IC , and critical energy release rate G C compared to pure 2D COFs. This enhancement is likely due to the graphene layers as the backbone of the sandwich structure effectively carrying and redistributing mechanical stress within the nanocomposite. Our findings demonstrate that a sandwich structure can improve the mechanical robustness of a 2D COF so that it can preserve the functionality and mechanical integrity for applications in stretchable electronics.

36 MATERIALS SCIENCE↗