Fast Thermal Cycling Research Articles

Thermal, Microstructural, and Mechanical Analysis of Complex Lattice Structures Produced by Direct Energy Deposition.

Lattice structures have gained attention in engineering due to their lightweight properties. However, the complex geometry of lattice structures and the high melting temperature of metals present significant manufacturing challenges for the large-scale fabrication of these structures. Direct Energy Deposition (DED) methods, such as the Wire Arc Additive Manufacturing (WAAM) technique, appear to be an interesting solution for overcoming these limitations. This study provides a detailed analysis of the manufacturing process of carbon steel lattice structures with auxetic geometry. The study includes thermal analysis using infrared thermography, microstructural characterization through metallography, and mechanical evaluation via hardness and mechanical testing. The findings reveal the significant impact of heat input, thermal cycles, and deposition sequence on the morphology and mechanical properties of the lattice structures. Fast thermal cycles are related to areas with higher hardness values, smaller strut diameters, and porous formations, which shows that controlling heat input and heat dissipation is crucial for optimizing the properties of lattice structures produced using WAAM.

Reliability of VO textsubscript 2-Based mmWave Switches Under 100 Million Thermal Cycles

We report the lifetime investigations of the reversible phase transition vanadium dioxide (VO2) thin film switches integrated with coplanar waveguide (CPW) under fast and direct thermal cycling. We observe that after 100 million thermal cycles, there is no degradation in the performance of VO2 shunt switches operating at 35 – 45 GHz. S11 reflection coefficient as well as S21 transmission measurements (verified independently at both activated and inactivated states) show no statistical difference in port-to-port coupling of the VO2 switch as a function of a cycle number. This study is enabled by the integration of Joule heaters on chip at a close proximity to a shunt VO2 switch and a metallic CPW transmission line. Full-wave electromagnetic and multiphysics electrothermal finite element simulations are conducted to analyze the feasibility of the CPW design and the required time and power for thermal cycling. On-wafer mmWave measurements are carried out on the test vehicle after each thermal cycling phase.

Fabrication, property and performance evaluation of Stainless Steel 430L as porous supports for metal supported solid oxide fuel cells

Metal-supported solid oxide fuel cells (MS-SOFCs) have attracted increasing attention due to their superior mechanical strength, relatively low material cost, and capability of fast thermal cycling, as compared to the conventional all-ceramic solid oxide fuel cell. However, fabrication of MS-SOFCs still remains challenging. This study reports a cost-effective powder metallurgical manufacturing route for producing MS-SOFCs. Stainless steel 430L (SS430L) powder is selected for producing the metal support due to its relatively low cost and good thermal expansion compatibility. MS-SOFC button cells with the SS430L/YSZ|Ni/YSZ|YSZ|LSCF structure were successfully prepared by co-sintering and ultrasonic pyrolytic spraying. We found that the trace oxygen level in the dilute H2/Ar gas mixture could play a drastic role in laboratory sintering of the SS430L support; local oxygen control is essential, particularly to avoid Cr oxidation. The addition of no more than 10% YSZ as a second phase to SS430L substantially minimized over-sintering of the SS430L support, leading to a more porous metallic-type substrate, while the electrical conductivity and thermal expansion were not much affected. The fabricated MS-SOFC button cells with the SS430L/YSZ|Ni/YSZ|YSZ|LSCF structure delivered a maximum power density of 180 mW cm-2 at 800°C with an open-circuit voltage of 1.13 V, using dry hydrogen as the fuel and ambient air as an oxidant. A cell tested at 750°C showed relatively good stability for a period of 140 h. While the performance still needs further optimization, the high OCV and good stability indicated that the reported powder metallurgy route is a promising method, and the relevant experimental details, particularly on producing metallic and oxidation-free porous supports, are critical for the preparation of MS-SOFCs.

Decarburization in Laser Surface Hardening of AISI 420 Martensitic Stainless Steel.

Decarburization deteriorates the surface mechanical properties of steel. It refers to the loss of carbon from steel's surface when exposed to an open-air environment in elevated-temperature conditions. Despite the short interaction time and fast thermal cycle of the laser surface-hardening process, decarburization may still occur. This paper investigates if decarburization occurs during the laser surface hardening of AISI 420 martensitic stainless steel. For comparison, surface-hardening results and decarburizations in a conventional air furnace-heated hardening process (water-quenched and air-cooled) of the same steel material were also investigated. Decarburization seems to have occurred in the laser surface hardening of AISI 420SS. However, the decarburization might not be significant, as the hardness of the steel's surface was increased more than three times to 675 HV during the laser surface hardening, and the hardness drop due to decarburization was estimated to be only 3% with the decarburization depth of 40 μm. Simulations using ThermoCalc software to get the carbon concentration profiles along the depth for both laser-hardened and furnace-heated samples were also investigated.

Linking Powder Properties, Printing Parameters, Post-Processing Methods, and Fatigue Properties in Additive Manufacturing of AlSi10Mg

Additive manufacturing (AM) of metals can be broadly accomplished via two defined technologies: powder bed fusion and directed energy deposition. During AM fabrication, the melted feedstock material experiences fast thermal cycling due to the layer-by-layer deposition process resulting in microstructures and properties that are drastically different from the traditionally manufactured parts. For AM to become a viable process for fabricating critical components made of high-performance structural alloys, such as AlSi10Mg, a comprehensive understanding is required toward developing the process-structure-property relationships prevalent in AM. AlSi10Mg, with its good castability, strength, hardness, and dynamic properties, is typically used to fabricate structural components that are required to withstand high loads. This alloy has been consolidated predominantly by the laser powder bed fusion (L-PBF) method and several critical mechanical properties, such as fatigue, have been reported to date. This article, first, summarizes the as-deposited and heat-treated microstructures of AlSi10Mg specimens fabricated by L-PBF. Then, the article discusses the linkages among the feedstock properties, printing parameters, specimen geometry, post-processing techniques, and fatigue properties. This discussion is followed by a section on the fatigue life prediction of AlSi10Mg specimens using computational modeling. Finally, the article identifies critical research gaps and pinpoints future research opportunities.

Microstructure evolution and tensile property of TiAl alloy using continuous direct energy deposition technique

Attributing to the fast solidification and thermal cycling during additive manufacturing process, massive phase transformation could take place thus leading to the formation of unpredictable microstructures with large variation in mechanical properties. In this paper, a continuous direct energy deposition technique (CDED) is adopted to prepare TiAl alloy seceding from the thermal cycling, and the evolution of microstructure, microhardness and tensile properties of alloy are investigated. Results indicate that the microstructure of alloy composes of columnar grains with very fine (α2 +γ) lamellae, and no heat-affect band is observed. A heat transfer model is established to assist in explaining the solid-phase transformation and microstructure formation mechanism of TiAl alloy. Furthermore, a special duplex γ microstructure (DP γ) forms which composes of massive γ phase surrounded by feathery-like γ phase. By dissecting crystallographic orientation from EBSD results, the formation mechanism of DP γ is clarified as the result of sequential solid-state phase transition in (α + γ) phase region, in which the feathery-like microstructure forms firstly followed by the massive γ phases nucleating at the inter-phase boundaries of feathery-like γ. Tensile property of as-deposited alloy reveals of 535 MPa with 1% elongation, and the highest hardness of around 320HV is detected at the top region of alloy with the finest interlamellar spacing.

Degradation Mechanisms of Solid Oxide Fuel Cells under Various Thermal Cycling Conditions.

A critical issue to tackle before successful commercialization of solid oxide fuel cells (SOFCs) can be achieved is the long-term thermal stability required for SOFCs to operate reliably without significant performance degradation despite enduring thermal cycling. In this work, the impact of thermal cycling on the durability of NiO-yttria-stabilized zirconia-based anode-supported cells is studied using three different heating/cooling rates (1, 2, and 5 °C min-1) as the temperature fluctuated between 400 and 700 °C. Our experiments simulate time periods when power from SOFCs is not required (e.g., as might occur at night or during an emergency shutdown). The decay ratios of the cell voltages are 8.8% (82 μV h-1) and 19.1% (187 μV h-1) after thermal cycling testing at heating/cooling rates of 1 and 5 °C min-1, respectively, over a period of 1000 h. The results indicate SOFCs that undergo rapid thermal cycling experience much greater performance degradation than cells that experience slow heating/cooling rates. The changes in total resistance for thermally cycled cells are determined by measuring the Rpol of the electrodes (whereas the ohmic resistances of the cells remain unchanged from their initial value), signifying that electrode deterioration is the main degradation mechanism for SOFCs under thermal cycling. In particular, fast thermal cycling leads to severe degradation in the anode part of SOFCs with substantial agglomeration and depletion of Ni particles seen in our characterizations with field emission-scanning electron microscopy and electron probe microanalysis. In addition, the mean particle size in the cathode after thermal cycling testing increases from 0.104 to 0.201 μm for the 5 °C min-1 cell. Further, the presence of Sr-enriched regions is more significant in the La0.6Sr0.4Co0.2Fe0.8O3-δ cathode after fast thermally cycled SOFCs.

Portable Magnetofluidic Device for Point-of-Need Detection of African Swine Fever.

With a nearly 100% mortality rate, African swine fever (ASF) has devastated the pork industry in many countries. Without a vaccine in sight, mitigation rests on rapid diagnosis and immediately depopulating infected or exposed animals. Unfortunately, current tests require centralized laboratories with well-trained personnel, take days to report the results, and thus do not meet the need for such rapid diagnosis. In response, we developed a portable, sample-to-answer device that allows for ASF detection at the point of need in <30 min. The device employs droplet magnetofluidics to automate DNA purification from blood, tissue, or swab samples and utilizes fast thermal cycling to perform real-time quantitative polymerase chain reaction (qPCR), all within an inexpensive disposable cartridge. We evaluated its diagnostic performance at six farms and slaughter facilities. The device exhibits high diagnostic accuracy with a positive percent agreement of 92.2% and a negative percent agreement of 93.6% compared with a lab-based reference qPCR test.

Flexible and Modular Fully Metallic Housing Concept for Solid Oxide Fuel Cells

The state-of-the-art alumina oxide housings used in single cell test rigs are fragile, inflexible and expensive. They are designed for a specific cell geometry, a change of the cell type - changing the cell thickness - or a change in the cell size is not intended and is thus associated with an immense expenditure of effort and time. In detail, the state-of-the-art ceramic frame concept is vulnerable to a fracturing of the frame or an insufficient contacting of the cell if a change in the cell thickness occurs. The connection of the ceramic housing with the typically metallic tubing of the gas supply is fragile, prone to develop leakages and is time consuming to replace and thereby prevents a change of the cell size. Gold wire seals used at the cathode side are a common source of leakage. Furthermore, the whole ceramic housing is sensitive to fracturing due thermal or load induced stress, and thus prevents fast thermal cycling of the specimen.This paper presents a modular, fully metallic housing concept which enables a fast and easy change of the cell size due to the utilization of a baseplate and a robustness towards different cell thicknesses due to the usage of a flexible metallic frame. The utilization of metal instead of alumina oxide reduces the manufacturing costs. Furthermore, an additional sealing on the cathode side enables a separation of the contacting pressure via a pneumatic piston from the sealing pressure applied via metallic screws. The force of the sealing pressure is not applied onto the cell and is thereby limited by the material constraints and not by the mechanical stability of the cell. For accurate voltage measurements, sense wires are separated from the current collection and are electrically isolated from the metallic housing. Thermocouples are used to measure the temperature distribution inside the anodic part of the housing, as close as possible to the cell. The chromium evaporation of the cathode part of the housing is reduced by a protective coating and the utilization of double layered tubes. In the end, the results of preliminary tests are presented.

Thermal Behavior and Molten Pool Morphology during Laser 3D Printing Process of Alloy Steel Powder

In this paper, a finite element analysis (FEA) model is proposed to systematically study the thermal behavior of metal material in Selective Laser Melting (SLM) 3D printing process. It is found that the material undergoes a fast and complex thermal cycle process. Laser beam can re-heat the adjacent formed scanning track and layer, and also produce a certain preheating effect on the unformed powder bed of the adjacent scanning track when laser beam scans a track, which is conductive to improve metallurgical bonding performance of SLM-fabricated parts. With the increase of scanning tracks or scanning layers, the peak temperature and molten pool lifetime increase owing to the thermal accumulation effect, but the increasing trend gradually slows down. The peak temperature and lifetime of each scanning track center in the second layer are larger than those of the corresponding scanning tracks in the first layer, respectively. Furthermore, SLM experiments are carried out to study complicated molten pool morphology in SLM process. The results obtained in this study have certain guiding significance for understanding thermal mechanisms of SLM process.

Rapid identification of Babesia canis and Babesia gibsoni (Asian genotype) in canine blood samples using a customized portable real-time PCR analyzer and TaqMan-based assay

Canine babesiosis is a serious infectious disease in subtropical and tropical regions. Typically, clinical detection of canine babesiosis is performed by blood smear observation or the traditional polymerase chain reaction (PCR). Herein, we developed a new TaqMan-based real-time PCR assay combined with a customized portable real-time PCR platform for a rapid and accurate detection of canine babesiosis. Two new primer/probe pairs (B18S and BITS1) were designed based on 18S ribosomal RNA and an internal transcribed spacer 1 (ITS1) sequence to differentiate Babesia canis and B. gibsoni (Asian genotype) DNAs from canine blood samples. Additionally, a corresponding customized compact real-time PCR platform with low 6-carboxyfluorescein fluorescence detection (≤5 nM), including a fast and accurate thermal cycling ability with a user-friendly interface for thermal control and data analysis, was designed for the limited space use. Both assays (B18S and BITS1) demonstrated a sensitivity of 100 copies/reaction based on the 95 % confidence interval evaluation method. The self-developed customized portable real-time PCR analyzer presented high repeatability and reproducibility with the TaqMan-based assay. Moreover, 501 clinical specimens were collected for evaluating the performance of the proposed PCR. The positive and negative predictive values were 90 % (18 of 20) and 100 % (226 of 226), respectively, for samples suspected with B. canis infection and 98 % (55 of 56) and 100 % (199 of 199), respectively, for samples suspected with B. gibsoni infection.

Small-Size Polymerase Chain Reaction Device with Improved Heat Transfer and Combined Feedforward/Feedback Control Strategy

We report improvements on the heat transfer and on the control strategy of a thermal cycler implemented on a novel device for performing a fast polymerase chain reaction (PCR). The reduction of the thermal mass of the sample holder and the direct contact with the sample allow for a significant reduction of the transition times, while the hybrid feedforward/feedback controller can rely on inexpensive components (actuators, sensors, processor) and still achieve minimal over/undershooting and good temperature stability. The design of the device has been improved by performing transient heat conduction analysis on the highly heat-conductive sample holder and on the solid metal body of the device which rapidly dissipates the excess heat produced during the thermal cycling. In the current setup, the sample holder hosts nine 1 μL samples covered with mineral oil, which can be simultaneously read in real time by the detection module designed in-house and installed on the device. An increase in speed of the PCR amplification was achieved with a reduction of the transition time of 63.8% when compared against a commercial real-time PCR machine. Our work shows that a complete, stand-alone, and ready-to-use quantitative PCR instrument can be fabricated from inexpensive and easily available components and it can achieve fast thermal cycling thanks to a hybrid control strategy.

Design of next-generation ceramic fuel cells and real-time characterization with synchrotron X-ray diffraction computed tomography

Ceramic fuel cells offer a clean and efficient means of producing electricity through a variety of fuels. However, miniaturization of cell dimensions for portable device application remains a challenge, as volumetric power densities generated by readily-available planar/tubular ceramic cells are limited. Here, we demonstrate a concept of ‘micro-monolithic’ ceramic cell design. The mechanical robustness and structural integrity of this design is thoroughly investigated with real-time, synchrotron X-ray diffraction computed tomography, suggesting excellent thermal cycling stability. The successful miniaturization results in an exceptional power density of 1.27 W cm−2 at 800 °C, which is among the highest reported. This holistic design incorporates both mechanical integrity and electrochemical performance, leading to mechanical property enhancement and representing an important step toward commercial development of portable ceramic devices with high volumetric power (>10 W cm−3), fast thermal cycling and marked mechanical reliability.

The effect of cold work on the transformation kinetics and texture of a zirconium alloy during fast thermal cycling

The effect of cold-work on the transformation kinetics and texture evolution after fast temperature cycling were studied in a dilute zirconium alloy. It was found that cold-work delays the onset of phase transformation and helps randomise the texture after the transformation. Samples of Zircaloy-4 in two conditions, cold-rolled to 70% reduction and fully recrystallised, were heated above the β-transus at a fast rate of 100 °C s−1 using resistive heating and without constraint. Electrical resistivity was used to measure the phase fraction during heating and electron back-scatter diffraction was used to measure the texture before and after the thermal cycle. Whereas previous work on titanium suggested that cold-work leads to texture strengthening after transformation, these new experiments show that, when the heating rate is fast enough, recrystallisation is incomplete on heating, which slows down the start of transformation, leading to a random α-texture after cooling. The texture in the recrystallised material after β heat-treatment is non-random but different from the start, a consequence of both a stronger β-texture after grain growth and stronger variant selection on cooling. This variant selection can be mostly explained by α-nucleation at special β-grain boundaries. These results demonstrate that prior deformation has a strong effect on the textures produced after β-heat treatment when heating rates are fast. This has implications for the anisotropy of nuclear cladding components after loss-of-coolant (LOCA) and reactivity-initiated accidents (RIA) but also more widely for the manufacturing of zirconium and titanium using welding or additive layer manufacturing where the heating rates are high.

Frequency domain analysis of pyroelectric response in silicon-doped hafnium oxide (HfO2) thin films

The pyroelectric response of polycrystalline, Si-doped HfO2 layers with a thickness of 20 nm is investigated in a frequency range of 2 Hz to 20 kHz. Local Joule heating of the pyroelectric material by a deposited nickel strip is used to achieve fast thermal cycles. Over the whole frequency range, a distinct pyroelectric response is registered. A pyroelectric coefficient of −72 μC/m2K is obtained at a frequency of 10 Hz, which is in good agreement with earlier low-frequency measurements. The pyroelectric current is evaluated with respect to electric field cycling, where a successive increase is observed during wake-up. By comparing measurement results in the low- and high-frequency limit, primary and secondary pyroelectric coefficients of −53 μC/m2K and −19 μC/m2K are estimated, respectively. Si-doped HfO2 is a promising material for future energy harvesting and IR sensor applications due to environmental friendliness and CMOS compatible manufacturing.

A simple metal-semiconductor substructure for the advanced thermo-mechanical numerical modeling of the power integrated circuits

The metallization of double-diffused metal-oxide semiconductor (DMOS) power devices, which operate under fast thermal cycling (FTC), undergoes thermal induced plastic metal deformation (TPMD). The design of the metallization has a significant impact on the device lifetime and thus requires a thorough understanding of the temperature, stress and strain distribution. A simple three-dimensional (3D) transistor substructure which is commonly found in various high integration Bipolar-CMOS-DMOS (BCD) technologies is analysed. The thermomechanical behaviour is studied with the finite element method (FEM) for investigation of two potential failure mechanisms: delamination of power metal and accumulation of plastic deformation in signal metallization layer (which leads to inter-metal dielectric cracking). These failure mechanisms are analysed on two versions of the structure: the first one has only signal and power metal lines and the second one has vias, in addition to the signal and power metal lines. The target of the paper is to propose an efficient finite element analysis (FEA) model that can be used for a qualitative assessment of thermo-mechanical phenomena in the metal system of high integration BCD technologies.

Developmental validation of GlobalFiler\u2122 PCR amplification kit: a 6-dye multiplex assay designed for amplification of casework samples

The GlobalFiler™ PCR Amplification Kit is a single multiplex assay that amplifies a set of 24 markers, which encompass the European Standard Set and CODIS (Combined DNA Index System) recommended composite set of loci. In addition to more loci and a 6-dye chemistry format, the Master Mix has been formulated to allow higher sample loading volume for trace DNA samples. The GlobalFiler™ Kit has been optimized to deliver high performance on casework samples, while also delivering fast thermal cycling, with an amplification time of approximately 80 min. Here, we report the results of the developmental validation study which followed the SWGDAM (Scientific Working Group on DNA Analysis Methods) guidelines and includes data for PCR-based studies, sensitivity, species specificity, stability, precision, reproducibility and repeatability, concordance, stutter, DNA mixtures, and performance on mock casework samples. The results validate the multiplex design as well as demonstrate the kit’s robustness, reliability, and suitability as an assay for human identification with casework DNA samples.

Highly Precise and Fast Polymerase Chain Reaction Thermal Cycling Module with a Novel Integrated Temperature Control Strategy

Highly Precise and Fast Polymerase Chain Reaction Thermal Cycling Module with a Novel Integrated Temperature Control Strategy

Durability of symmetric-structured metal-supported solid oxide fuel cells

Symmetric-structure metal-supported solid oxide fuel cells (MS-SOFC) with YSZ electrolyte are fabricated with porous YSZ backbone electrodes, stainless steel supports, and infiltrated catalysts on both anode and cathode side. Durability towards aggressive thermal and redox cycling, and long-term operation is assessed. Many sealing material candidates are screened for compatibility with the cell materials and operating conditions, and a commercial sealing glass, GM31107, is selected. LSM/SDCN cells are then subjected to 200 very fast thermal cycles and 20 complete redox cycles, with minimal impact to cell performance. LSM/SDCN and SDCN/SDCN cells are operated for more than 1200 h at 700 °C. The seal and cell hermeticity is maintained, and cell ohmic impedance does not change significantly during operation. Electrode polarization increases during operation, leading to significant degradation of the cell performance. In-operando EIS and post-mortem SEM/EDS analysis suggest that catalyst coarsening and cathode Cr deposition are the dominant degradation modes.

Accelerated aging of fast thermal cycle effects on the behavior of space charge in polyimide

The spacecraft often interacts with plasma, high energy particles and magnetic fields on orbit. It causes the charge injected in the insulation materials and forms a high electric field. The discharge phenomenon will happen when the internal electric field reaches the discharge voltage threshold. The insulation material is a key component of electrical equipment on the spacecraft, its electrical properties affects the reliability and lifetime of the whole spacecraft. The insulation material on spacecraft withstands fast thermal cycle during operation on orbit, which causes internal thermal stress in it. The accumulation of internal thermal stress changes the material molecular structure and depolarization characteristics, thus affecting the behavior of the space charge inside the insulation material. In this paper, the temperature environment was achieved by contact heating plant and liquid nitrogen immersion to do accelerated aging test based on the temperature of operating spacecraft. By the mean of this method, 0, 50, 100, 150 and 200 times of the fast thermal cycle was carried out. The molecular structure characteristics, the thermally stimulated current characteristics and the space charge characteristics of the samples with different cycling times were studied through the methods including XPS, XRD, TSC and PEA. The results show that with the increase of fast thermal cycling times, the relative content of the C-N and C=O bonds increase and it also increases the shallow energy level charges. The charges are more easily to move inside the sample. Fast thermal cycle also increases the degree of crystallinity, thus the interface between crystalline region and amorphous region expands. It also increases the charge of deep energy level, which increased the amount of space charge injected in the sample.