Pyroelectric Thin films for gas sensing
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Luk, Ting S.↗
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Wake-up and fatigue mechanisms in ferroelectric Hf 0.5 Zr 0.5 O 2 films with symmetric RuO 2 electrodes
In this work, the mechanisms leading to wake-up and fatigue in ferroelectric hafnium zirconium oxide thin film devices with symmetric RuO 2 electrodes are investigated via polarization, relative permittivity, dielectric nonlinearity, pyroelectric coefficient, and microfocus X-ray diffraction (XRD) measurements. The devices are observed to wake-up for up to 10 3 bipolar pulsed field cycles, after which fatigue occurs with the polarization approaching zero following 10 8 cycles. Wake-up is accompanied by a decrease in both high-field permittivity and hysteresis loop pinching and an increase in pyroelectric coefficient, indicating that the wake-up process involves a combination of transformations from the tetragonal to the orthorhombic phase and domain depinning from defect redistribution. Fatigue is observed to coincide with an increase in irreversible domain wall motion and a decrease in pyroelectric coefficient. Finite pyroelectric coefficients are measured on fully fatigued devices, indicating that domain pinning is a strong contributor to fatigue and that fatigued devices contain domain structures that are unable to switch under the fields applied for measurement. Microfocus XRD patterns measured on each device reveal that the phase constitution is qualitatively unaffected by the field cycling and resultant polarization fatigue. This data indicates that the wake-up process has contributions from both phase transformations and domain depinning, whereas the fatigue process is driven primarily by domain pinning, and the near-zero measured switchable polarization is actually a poled device with immobile domains. These observations provide insight into the physical changes occurring during field cycling of HfO 2 -based ferroelectrics while examining a possible oxide electrode material for silicon CMOS device implementation.
75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
High Efficiency Waste Heat Harvesting Using Novel Thermal Oscillators
The aim of this project was to enable practical energy generation from waste heat using pyroelectric (PE) materials with unprecedented efficiency. This aim was accomplished by engineering novel heat switches that overcome the current roadblock to pyroelectric energy harvesting. The heat switches produce a sustain temporal temperature differences from a constant flux heat source. Pyroelectric materials produce transient voltages in response to this generated temperature oscillation. The project solved the inability to generate sustained temperature cycles by utilizing LCEs to achieve passive thermal switching, or EDH of thermal fluid to actively bridging/de-bridging between heat source and pyroelectric layer.
30 DIRECT ENERGY CONVERSION↗
Low cost space power generation
The success of this study has given a method of fabricating durable copolymer films without size limitations. Previously, only compression molded samples were durable enough to generate electrical energy. The strengthened specimens are very long lived materials. The lifetime was enhanced at least a factor of 1,300 in full pyroelectric conversion cycle experiments compared with extruded, non-strengthened film. The new techniques proved so successful that the lifetime of the resultant copolymer samples was not fully characterized. The lifetime of these new materials is so long that accelerated tests were devised to probe their durability. After a total of more than 67 million high voltage electrical cycles at 100 C, the electrical properties of a copolymer sample remained stable. The test was terminated without any detectable degradation to allow for other experiments. One must be cautious in extrapolating to power cycle performance, but 67 million electrical cycles correspond to 2 years of pyroelectric cycling at 1 Hz. In another series of experiments at reduced temperature and electrical stress, a specimen survived over one-third of a billion electrical cycles during nearly three months of continuous testing. The radiation-limited lifetimes of the copolymer were shown to range from several years to millions of years for most earth orbits. Thus, the pyroelectric copolymer has become a strong candidate for serious consideration for future spacecraft power supplies.
Olsen, Randall B.↗
Systems and methods for wireless temperature sensing
Wireless temperature sensing systems and methods include an active sensor for determining temperature parameters in harsh environments, such as in very high temperature conditions, and wireless conveyance of the detected parameters. In an example embodiment, a pyroelectric element can generate a voltage when subjected to a temperature change. A coil is electrically coupled to the pyroelectric element and configured to generate a magnetic field in response to a current induced by the voltage generated by the pyroelectric element. A pickup is electromagnetically coupled with and detects the magnetic field generated by the coil, and the pickup is configured to provide an output corresponding to the detected magnetic field.
Lin, Yirong↗
Chapter 3 - Harvesting Thermal Energy with Ferroelectric Materials
Thermal energy is considered the ubiquitous form of energy as all other forms of energy ultimately degrade to thermal energy. Thermal to electrical energy conversion is currently an important method for electricity generation. The traditional power cycles, however, become technically and economically unviable when heat source temperature reduces below 100 °C. Thermal energy harvesting has been proposed as a viable alternative for low-grade thermal to electrical energy conversion. Thermal energy harvesting is a method of generating electricity using temperature-induced variations in material properties. It is particularly useful when the heat sources are available free-of-cost, either in the form of natural heat or waste heat. While there are several thermal energy harvesting techniques, pyroelectricity is the most promising as it can be used in situations where spatial thermal gradients are difficult to establish or the temperature of the heat source is changing. Despite the fact that the pyroelectric effect in ferroelectric materials has been known for past several decades, thermal energy harvesting using ferroelectric materials has not been much explored in the literature. In this chapter, we would explore various aspects of thermal energy harvesting using ferroelectric materials. We have first established the physics behind ferroelectricity, then provided a detailed description on ferroelectric thermal energy harvesting, discussed various ferroelectric thermodynamic cycles and devices proposed in the literature, and finally described various other emerging applications of ferroelectricity.
DIRECT ENERGY CONVERSION,MATERIALS SCIENCE,OTHER I↗
Broad Distribution of Local Polar States Generates Large Electrothermal Properties in Pb-Free Relaxor Ferroelectrics
Electrothermal energy conversion provides attractive solutions for global energy management, such as energy harvesting from waste heat using pyroelectric energy conversion (PEC) and efficient cooling of portable electronics or data servers using the electrocaloric effect. Relaxor ferroelectrics are attractive for electrothermal energy conversion because of their large pyroelectric coefficients over a wide temperature range. Although Pb-based relaxors are well-known, toxicity concerns have mandated the intense search for Pb-free alternatives. Here, we engineered (Ba,Ca)TiO 3 -based relaxors based on a multisite doping strategy, which show promising electrothermal performance, viz. a maximum PEC efficiency of 14% and electrocaloric refrigeration capacity of 115 J/kg. Using local-scale structural analysis, we provide an atomistic model for large electrothermal properties in the newly designed Pb-free ferroelectrics, whereby a temperature-independent continuous distribution of cation displacement directions creates easy pathways for microscopic polarization reorientation. This research provides key structural insight for future atomic-scale engineering of environmentally sustainable ferroelectrics in energy applications.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
High Entropy Oxide Relaxor Ferroelectrics
Relaxor ferroelectrics are important in technological applications due to strong electromechanical response, energy storage capacity, electrocaloric effect, and pyroelectric energy conversion properties. Current efforts to discover and design materials in this class generally rely on substitutional doping as slight changes to local compositional order can significantly affect the Curie temperature, morphotropic phase boundary, and electromechanical responses. In this work, we demonstrate that moving to the strong limit of compositional complexity in an ABO 3 perovskite allows stabilization of relaxor responses that do not rely on a single narrow phase transition region. Entropy-assisted synthesis approaches are utilized to synthesize single-crystal Ba(Ti 0.2 Sn 0.2 Zr 0.2 Hf 0.2 Nb 0.2 )O 3 [Ba(5B)O] films. The high levels of configurational disorder present in this system are found to influence dielectric relaxation, phase transitions, nanopolar domain formation, and Curie temperature. Temperature-dependent dielectric, Raman spectroscopy, and second-harmonic generation measurements reveal multiple phase transitions, a high Curie temperature of 570 K, and the relaxor ferroelectric nature of Ba(5B)O films. The first-principles theory calculations are used to predict possible combinations of cations to design relaxor ferroelectrics and quantify the relative feasibility of synthesizing these highly disordered single-phase perovskite systems. Further, the ability to stabilize single-phase perovskites with various cations on the B-sites offers possibilities for designing high-performance relaxor ferroelectric materials for piezoelectric, pyroelectric, and electrocaloric applications.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Resolving the Heat of Trimethylaluminum and Water Atomic Layer Deposition Half-Reactions
We report that atomic layer deposition (ALD) is a surface synthesis technique that is characterized by self-limiting reactions between gas-phase precursors and a solid substrate. Although ALD processes have been demonstrated that span the periodic table, a greater understanding of the surface chemistry that affords ALD is necessary to enable greater precision, including area- and site-selective growth. We offer new insight into the thermodynamics and kinetics of the trimethylaluminum (TMA) and H 2 O ALD half-reactions with calibrated and time-resolved in situ pyroelectric calorimetry. The half-reactions produce 3.46 and 2.76 eV/Al heat, respectively, which is greater than the heat predicted by computational models based on crystalline Al 2 O 3 substrates and closely aligned with the heat predicted by standard heats of formation. The pyroelectric thin-film calorimeter offers submilisecond temporal resolution that uniquely and clearly resolves precursor delivery and reaction kinetics. Both half-reactions are observed to exhibit multiple kinetic rates, with average TMA half-reaction rates at least 2 orders of magnitude faster than the H 2 O half-reaction kinetics. Comparing the experimental heat with published computational literature and additional first-principles modeling highlights the need to refine our models and mechanistic understanding of even the most ubiquitous ALD reactions.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Atomic lift-off of epitaxial membranes for cooling-free infrared detection
Recent breakthroughs in ultrathin, single-crystalline, freestanding complex oxide systems have sparked industry interest in their potential for next-generation commercial devices. However, the mass production of these ultrathin complex oxide membranes has been hindered by the challenging requirement of inserting an artificial release layer between the epilayers and substrates. Here we introduce a technique that achieves atomic precision lift-off of ultrathin membranes without artificial release layers to facilitate the high-throughput production of scalable, ultrathin, freestanding perovskite systems. Leveraging both theoretical insights and empirical evidence, we have identified the pivotal role of lead in weakening the interface. This insight has led to the creation of a universal exfoliation strategy that enables the production of diverse ultrathin perovskite membranes less than 10 nm. Our pyroelectric membranes demonstrate a record-high pyroelectric coefficient of 1.76 × 10 −2 C m −2 K −1 , attributed to their exceptionally low thickness and freestanding nature. Moreover, this method offers an approach to manufacturing cooling-free detectors that can cover the full far-infrared spectrum, marking a notable advancement in detector technology.
nanoscale materials↗
Relaxor behavior and electrothermal properties of Sn- and Nb-modified (Ba,Ca)TiO 3 Pb-free ferroelectric
Relaxor ferroelectrics have drawn attention for possible applications in solid-state cooling and thermal energy harvesting, owing to their electrothermal energy conversion properties. Here, we have synthesized and characterized the structure–property correlations of a new Sn- and Nb-doped (Ba,Ca)TiO 3 relaxor ferroelectric with large pyroelectric and electrocaloric effects over a broad temperature range. We observed two peaks for the temperature-dependent pyroelectric coefficient: (i) -(∂P/∂T) ~ 563 µC/(m 2 K) at T~ 270 K and (ii) -(∂P/∂T) ~ 1021 µC/(m 2 K) at T~ 320 K. In addition, a broad peak for electrocaloric temperature change is observed near 320 K with a relative cooling power of ~17 J/kg. These properties could be correlated to structural changes observed using X-ray diffraction at two different temperature ranges in the material. Analysis of high-energy X-ray scattering and specific heat capacity data revealed a transition from the cubic to tetragonal phase near T m ~ 320 K, whereas an additional increase in the tetragonality (c/a) of the polar phase is observed below T s ~ 270 K.
36 MATERIALS SCIENCE↗
Compact carbon monoxide sensor utilizing a confocal optical cavity.
The carbon monoxide sensor discussed in this paper utilizes a unique confocal cavity which allows the complete system to be packaged in a small volume suitable for hand-held use. The optical system is the heart of the instrument with equal emphasis placed on the electronics support circuitry, consisting essentially of a thermal infrared pyroelectric detector and lock-in amplifier. The pyroelectric detector offers a major advantage over other thermal detectors, providing a signal-to-noise ratio and detectivity that remain nearly constant over the frequency range from dc to 2000 Hz. Since bias voltage is not required, low frequency noise is not generated in the detector.
Scott, B.↗
Detection of long wavelength infrared at moderate temperatures
Technical approaches for the advanced development of 8-12 micrometer detectors operating at elevated temperatures were defined. The theoretical limits to performance of 8-12 micrometer quantum detectors (photoconductive and photovoltaic) and thermal detectors (pyroelectrics, bolometers etc). An analytic model of signal and noise in both quantum detectors and pyroelectric detectors was developed and candidate materials for both detector types were identified and examined. The present status of both quantum and thermal detectors was assessed as well as the parameters limiting operating temperature and detectivity. The areas of research and development likely to lead to detector performance near the theoretical limit are identified.
Tredwell, T. J.↗
Magneto-inductive skin sensor for robot collision avoidance: A new development
Safety is a primary concern for robots operating in space. The tri-mode sensor addresses that concern by employing a collision avoidance/management skin around the robot arms. This rf-based skin sensor is at present a dual mode (proximity and tactile). The third mode, pyroelectric, will complement the other two. The proximity mode permits the robot to sense an intruding object, to range the object, and to detect the edges of the object. The tactile mode permits the robot to sense when it has contacted an object, where on the arm it has made contact, and provides a three-dimensional image of the shape of the contact impression. The pyroelectric mode will be added to permit the robot arm to detect the proximity of a hot object and to add sensing redundancy to the two other modes. The rf-modes of the sensing skin are presented. These modes employ a highly efficient magnetic material (amorphous metal) in a sensing technique. This results in a flexible sensor array which uses a primarily inductive configuration to permit both capacitive and magnetoinductive sensing of object; thus optimizing performance in both proximity and tactile modes with the same sensing skin. The fundamental operating principles, design particulars, and theoretical models are provided to aid in the description and understanding of this sensor. Test results are also given.
Chauhan, D. S.↗
Growth and characterization of crystals for room temperature I.R. detectors and second harmonic generation devices
One of the major objectives of this program was to modify the triglycine sulfate (TGS) crystals with suitable dopants and variants to achieve better pyroelectric properties and improved infrared detectivities (D(sup *)), and higher Curie transition temperature compared to undoped TGS crystals. Towards these objectives, many promising dopants, both inorganic and organic, were investigated in the last few years. These dopants gave significant improvement in the D(sup *) value of the infrared detectors fabricated from the grown crystals with no significant increase in the Curie temperature (49 C). The IR detectors were fabricated at EDO/Barnes Engineering Division, Shelton, CT. In the last one year many TGS crystals doped with urea were grown using the low temperature solution crystal growth facility. It is found that doping with urea, the normalized growth yield increased significantly compared to pure TGS crystals and there is an improvement in the pyroelectric and dielectric constant values of doped crystals. This gave a significant increase in the materials figure of merits. The Vicker's hardness of 10 wt percent urea doped crystals is found to be about three times higher in the (010) direction compared to undoped crystals. This report describes in detail the results of urea doped TGS crystals.
Lal, R. B.↗
Method of Making Thermally Stable, Piezoelectric and Proelectric Polymeric Substrates
A thermally stable, piezoelectric and pyroelectric polymeric substrate was prepared. This thermally stable, piezoelectric and pyroelectric polymeric substrate may be used to prepare electromechanical transducers, thermomechanical transducers, accelerometers, acoustic sensors, infrared sensors, pressure sensors, vibration sensors, impact sensors. in-situ temperature sensors, in-situ stress/strain sensors, micro actuators, switches, adjustable fresnel lenses, speakers, tactile sensors, weather sensors, micro positioners, ultrasonic devices, power generators, tunable reflectors, microphones, and hydrophones. The process for preparing these polymeric substrates includes: providing a polymeric substrate having a softening temperature greater than 100 C; depositing a metal electrode material onto the polymer film; attaching a plurality of electrical leads to the metal electrode coated polymeric substrate; heating the metal electrode coated polymeric substrate in a low dielectric medium: applying a voltage to the heated metal electrode coated polymeric substrate to induce polarization; and cooling the polarized metal electrode coated polymeric electrode while maintaining a constant voltage.
Simpson, Joycelyn O.↗