Evaluation of true interlamellar spacing from microstructural observations

A method for evaluating true interlamellar spacing from micrographs is proposed for a multidomained lamellar structure. The microstructure of these materials is assumed to be composed of many domains with the lamellae aligned roughly parallel to each other within each domain and with the domains themselves randomly oriented relative to one another. An explicit expression for the distribution of apparent interlamellar spacing is derived assuming that the distribution of the true interlamellar spacing is Gaussian. The average interlamellar spacing is close to the peak interlamellar spacing observed in the distribution. The theoretical distributions are compared with experimental ones obtained by analyzing micrographs of PbTe–Sb2Te3 lamellar composites

Lattice thermal conductivity of self-assembled PbTe-Sb_2Te_3 composites with nanometer lamellae

In the system of PbTe and Sb_2Te_3, a metastable compound Pb_2Sb_6Te_(11) appears by solidification processing. It has been reported that this compound is decomposed into the two immiscible thermoelectric materials forming nanosized lamellar structure by heat treatments. The fraction transformed and the inter-lamellar spacing was systematically investigated. In this work, the thermal conductivities and the electrical resistivities have been measured as functions of annealing time through the transformation and the coarsening processes to clarify the effect of the fraction transformed and the inter-lamellar spacing. The thermal conductivity of Pb_2Sb_6Te_(11) is lower than that after the decomposition. The lattice part of the thermal conductivity of PbTe/Sb_2Te_3 lamellar samples decreases with decreasing inter-lamellar spacing. This is considered to be due to the coarsening of the microstructure

Fabrication of Lanthanum Telluride 14-1-11 Zintl High-Temperature Thermoelectric Couple

The development of more efficient thermoelectric couple technology capable of operating with high-grade heat sources up to 1,275 K is key to improving the performance of radioisotope thermoelectric generators. Lanthanum telluride La3-xTe4 and 14-1-11 Zintls (Yb14MnSb11) have been identified as very promising materials. The fabrication of advanced high-temperature thermoelectric couples requires the joining of several dissimilar materials, typically including a number of diffusion bonding and brazing steps, to achieve a device capable of operating at elevated temperatures across a large temperature differential (up to 900 K). A thermoelectric couple typically comprises a heat collector/ exchanger, metallic interconnects on both hot and cold sides, n-type and ptype conductivity thermoelectric elements, and cold-side hardware to connect to the cold-side heat rejection and provide electrical connections. Differences in the physical, mechanical, and chemical properties of the materials that make up the thermoelectric couple, especially differences in the coefficients of thermal expansion (CTE), result in undesirable interfacial stresses that can lead to mechanical failure of the device. The problem is further complicated by the fact that the thermoelectric materials under consideration have large CTE values, are brittle, and cracks can propagate through them with minimal resistance. The inherent challenge of bonding brittle, high-thermal-expansion thermoelectric materials to a hot shoe material that is thick enough to carry the requisite electrical current was overcome. A critical advantage over prior art is that this device was constructed using all diffusion bonds and a minimum number of assembly steps. The fabrication process and the materials used are described in the following steps: (1) Applying a thin refractory metal foil to both sides of lanthanum telluride. To fabricate the n-type leg of the advanced thermoelectric couple, the pre-synthesized lanthanum telluride coupon was diffusion bonded to the metal foil using a thin adhesion layer. (2) Repeating a similar process for the 14-1-11 Zintl p-type leg of the advanced thermoelectric couple. (3) Bonding thick CTE-matched metal plates on the metallized lanthanum telluride and Yb14MnSb11 to form the hot and cold sides of the thermoelectric couple. The calculated conversion efficiency of such an advanced couple would be about 10.5 percent, about 35 percent better than heritage radioisotope thermoelectric technology that relies on Si-Ge alloys. In addition, unlike Si-Ge alloys, these materials can be combined with many other thermoelectric materials optimized for operation at lower temperatures to achieve conversion efficiency in excess of 15 percent (a factor of 2 increase over heritage technology)

Solidification processing of Te-Sb-Pb alloys for thermoelectric applications

A solidification processing approach to the refinement of lead-tellurium-antimony alloy microstructure is described. Liquid alloys with eutectic, hyper-eutectic and hypo-eutectic compositions (relative to lead) were cooled to the solid state in three distinct ways, i.e. by water quenching, air cooling and furnace cooling. The structures of the alloys resulting from the three different solidification paths were examined using electron microscopy and the micrographs were quantified. Classical solidification methods were used to interpret the structures in relation to the cooling histories

Ultra-Light Ultra-Strong Proppants

The present invention provides a method of preparing a proppant material by heating a reaction mixture comprising a plurality of oxides in a reactive atmosphere to a temperature above the melting point of the reaction mixture to form a melt, and then allowing the melt to solidify in a mold in the form of spherical particles. The present invention also provides a method of preparing a proppant material by heating a reaction mixture comprising a plurality of oxides and one or more additives in a reactive atmosphere to a temperature below the melting point of the reaction mixture to form a powder including one or more reaction products, and then processing the powder to form spherical particles. The present invention also provides a proppant material including spherical particles characterized by a specific gravity of about 1.0 to 3.0 and a crush strength of at least about 10,000 psi

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

Formation of Sb_2Te_3 Widmanstätten precipitates in thermoelectric PbTe

Unidirectional solidification experiments have been performed with a thermoelectric alloy with a starting composition of Pb_(10.5)Sb_(31.6)Te_(57.9) in the pseudobinary PbTe–Sb_2Te_3 system. The bottom of the resulting rod consists of PbTe phase with Widmanstätten precipitates of Sb_2Te_3. The precipitation is due to a decrease in the solubility of Sb_2Te_3 with temperature: the solubility at 450 °C was determined to be 2.1 ± 0.2 at.% Sb. The average thickness of plates was estimated to be ~100 nm. The spacings between neighboring plates has a distribution in the 200–3000 nm range, peaking around 900 nm. The habit planes of precipitation are of the {111}PbTe family. An orientation relationship of (0001)Sb_2Te_3//{111}PbTe and Sb_2Te_3//PbTe was found with a maximum misorientation of 15°. The Seebeck coefficient after annealing at 450 °C was −50 ± 10 μV °C^−1 at room temperature. To improve the thermoelectric properties, tuning of the carrier concentration would be necessary

Microstructure Size Control through Cooling Rate in Thermoelectric PbTe-Sb_2Te_3 Composites

Microstructures of alloys with three compositions in the pseudobinary PbTe-Sb_2Te_3 system cast in copper molds using the injection molding technique were examined by scanning electron microscopy (SEM), energy-dispersive spectrometry, and X-ray diffraction (XRD). The microstructural length scales such as interlamellar spacing (ILS) and secondary dendrite arm spacing vary over two orders of magnitude, e.g., from 0.2 to 20 μm for SDAS in the hypereutectic alloy, depending on injection pressure, distance from surface, or thickness. The decrease in the microstructural length scale with the decrease in distance from the surface, thickness, and increase in injection pressure is attributed to an increase in the cooling rates estimated using the heat-transfer theory in solids. The difference in the injection pressures is represented as the difference in the heat-transfer coefficients