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Functional CeO x nanoglues for robust atomically dispersed catalysts
Single-atom catalysts make exceptionally efficient use of expensive noble metals and can bring out unique properties. However, applications are usually compromised by limited catalyst stability, which is due to sintering. Although sintering can be suppressed by anchoring the metal atoms to oxide supports, strong metal–oxygen interactions often leave too few metal sites available for reactant binding and catalysis, and when exposed to reducing conditions at sufficiently high temperatures, even oxide-anchored single-atom catalysts eventually sinter. Here we show that the beneficial effects of anchoring can be enhanced by confining the atomically dispersed metal atoms on oxide nanoclusters or ‘nanoglues’, which themselves are dispersed and immobilized on a robust, high-surface-area support. We demonstrate the strategy by grafting isolated and defective CeO x nanoglue islands onto high-surface-area SiO 2 ; the nanoglue islands then each host on average one Pt atom. Further, we find that the Pt atoms remain dispersed under both oxidizing and reducing environments at high temperatures, and that the activated catalyst exhibits markedly increased activity for CO oxidation. We attribute the improved stability under reducing conditions to the support structure and the much stronger affinity of Pt atoms for CeO x than for SiO 2 , which ensures the Pt atoms can move but remain confined to their respective nanoglue islands. The strategy of using functional nanoglues to confine atomically dispersed metals and simultaneously enhance their reactivity is general, and we anticipate that it will take single-atom catalysts a step closer to practical applications.
In-situ resource utilization in the design of advanced lunar facilities
Resource utilization will play an important role in the establishment and support of a permanently manned lunar base. At the University of Houston - College of Architecture and the Sasakawa International Center for Space Architecture, a study team recently investigated the potential use of lunar in-situ materials in the design of lunar facilities. The team identified seven potential lunar construction materials; concrete, sulfur concrete, cast basalt, sintered basalt, glass, fiberglass, and metals. Analysis and evaluation of these materials with respect to their physical properties, processes, energy requirements, resource efficiency, and overall advantages and disadvantages lead to the selection of basalt materials as the more likely construction material for initial use on a lunar base. Basalt materials can be formed out of in-situ lunar regolith, with minor material beneficiation, by a simple process of heating and controlled cooling. The team then conceptualized a construction system that combines lunar regolith sintering and casting to make pressurized structures out of lunar resources. The design uses a machine that simultaneously excavates and sinters the lunar regolith to create a cylindrical hole, which is then enclosed with cast basalt slabs, allowing the volume to be pressurized for use as a living or work environment. Cylinder depths of up to 4 to 6 m in the lunar mare or 10 to 12 m in the lunar highlands are possible. Advantages of this construction system include maximum resource utilization, relatively large habitable volumes, interior flexibility, and minimal construction equipment needs. Conclusions of this study indicate that there is significant potential for the use of basalt, a lunar resource derived construction material, as a low cost alternative to Earth-based materials. It remains to be determined when in lunar base phasing this construction method should be implemented.
Semiconductor structural damage attendant to contact formation in III-V solar cells
In order to keep the resistive losses in solar cells to a minimum, it is often necessary for the ohmic contacts to be heat treated to lower the metal-semiconductor contact resistivity to acceptable values. Sintering of the contacts, however can result in extensive mechanical damage of the semiconductor surface under the metallization. An investigation of the detailed mechanisms involved in the process of contact formation during heat treatment may control the structural damage incurred by the semiconductor surface to acceptable levels, while achieving the desired values of contact resistivity for the ohmic contacts. The reaction kinetics of sintered gold contacts to InP were determined. It was found that the Au-InP interaction involves three consecutive stages marked by distinct color changes observed on the surface of the Au, and that each stage is governed by a different mechanism. A detailed description of these mechanisms and options to control them are presented.
Bulk Grain-Boundary Materials from Nanocrystals
Grain-boundary engineering is pivotal to fully utilize the mechanical, electrical, and thermal-transport properties of various materials. However, current methods in metallurgy rely almost exclusively on top-down approaches, making precise grain-boundary engineering, especially at nanoscale, difficult to achieve. Herein, we report a method to produce tailored grain-boundary conditions with nanoscale precision from colloidal metal nanocrystals through surface treatment followed by a pressure-sintering process. The resulting bulk grain-boundary materials (which we call “nanocrystal coins”) possess a metal-like appearance and conductivity while inheriting the original domain features of the nanocrystal building blocks. In this work, nanoindentation measurements confirmed the superior mechanical hardness of the obtained materials. Further, we use this method to fabricate, for the first time, a single-component bulk metallic glass from amorphous palladium nanoparticles. Our discovery may spur the development of new materials whose functionality crucially depends on the domain configuration at nanoscale, such as superhard materials, thermoelectric generators, and functional electrodes.
Flux Synthesis of A-site Disordered Perovskite La 0.5 M 0.5 TiO 3 (M$=$Li, Na, K) Nanorods Tailored for Solid Composite Electrolytes
Inorganic fillers play an important role in improving the ionic conductivity of solid composite electrolytes (SCEs) for Li-ion batteries. Among inorganic fillers, perovskite-type lithium lanthanum titanate (LLTO) stands out for its high bulk Li + conductivity on the order of 10 -3 S cm -1 at room temperature. According to a literature survey, the optimal LLTO filler should possess the following characteristics: i) a single-crystal structure to minimize grain boundaries; ii) a small particle size to increase the filler/polymer interface area; iii) a 1D morphology for efficient interface channels; and iv) cubic symmetry to facilitate rapid bulk Li + diffusion within the filler. However, the synthesis of single crystal, 1D LLTO nanomaterials with cubic symmetry is challenging. Herein, a flux strategy is developed to synthesize La 0.5 M 0.5 TiO 3 (LMTO, M$=$Li, Na, and K) single-crystal nanorods with an A-site-disordered, cubic perovskite phase. The flux media promotes the oriented growth of nanorods, prevents nanorods from sintering, and provides multiple alkali metal ion doping at M sites to stabilize the cubic phase. SCEs compositing the Li + -conducting LMTO nanorods as fillers and poly[vinylene carbonate- co -lithium sulfonyl(trifluoromethane sulfonyl)imide methacrylate] matrix exhibit more than twice the conductivity of the neat polymer electrolyte (30.6 vs 14.0 µS cm -1 at 303 K).
Enhanced activity and stability of MgO-promoted Ni/Al 2 O 3 catalyst for dry reforming of methane: Role of MgO
Highly dispersed nickel nanoparticles (NPs) were deposited on Al 2 O 3 NPs by atomic layer deposition (ALD). Various amounts of MgO were loaded on Ni/Al 2 O 3 catalysts by the incipient wetness (IW) method for dry reforming of methane. Fresh and used catalysts were systematically characterized to reveal the effects of MgO on the catalytic performance. MgO was found to increase the basic amount and basic strength of catalyst surfaces, which provided additional surface oxygen species and assisted the adsorption and activation of CO 2 . Although the formation of NiO-MgO solid solution, during the calcination of incipient wetness, did not improve the overall reducibility, the Ni NPs from NiO-MgO solid solution after reduction formed an intimate interaction with MgO, which could inhibit Ni NPs from sintering and provide sufficient metal-support interface for CO 2 activation. The MgO-promoted Ni/Al 2 O 3 reached a methane reforming rate of 1780 L CH4 g Ni -1 h -1 at 850 °C, which is 26% more than that of the pristine Ni/Al 2 O 3 . Finally, the higher CO 2 activity enhanced the oxidation rate of the surface carbon generated from side-reactions, thereby resulting in a higher reforming rate and inhibiting coke formation, especially the detrimental graphitic encapsulating carbon on the active nickel surface.
Microhardness Distribution of Long Magnesium Block Processed through Powder Metallurgy
Powder metallurgy is a popular method of making raw powders into specific shaped samples. However, the pressure distribution and the microhardness difference within the sample are nonnegligible and unclear when the sample is long or exceeds a specific size. In this study, the long magnesium blocks, with a ratio of about 2.8 between the sample height and the sample side length, are successfully synthesized under three uniaxial and two biaxial conditions. Then, the sample hardness values on the outer surface and the center plane are tested to study the microhardness distribution. The modified analytical expression indicates that the normal pressure exponentially decreases along the compression direction, which is consistent with the hardness distribution trend. Because higher pressure leads to a more compact arrangement of the powders, more metal bonds are formed after sintering. During the first pressing, the sidewall pressure makes the surface hardness higher. The secondary reverse compression mainly improves the bottom and core hardness due to the re-orientation and re-location of the powders. The obtained relationship between the applied pressure and the hardness distribution is instructive in predicting and improving the sample quality.
A program to develop a high-energy density primary battery with a minimum of 200 watt hours per pound of total battery weight Sixth quarterly report, Oct. 1 - Dec. 31, 1965
Lithium anodes, inorganic and organic cathodes, vacuum-distilled solvents, and methods for sintering cupric fluoride on lightweight metal substrates - development of high energy battery
Nickel contacts for low cost solar cells
It is noted that nickel metallization of silicon solar cells offers a relatively inexpensive method of making electrical contact with the surface of the cell. More expensive methods, involving precious metals and costly processes, are widely used; these have been developed for space applications, where considerations of reliability predominate over those of cost. Since recent interest in terrestrial applications of solar cells has led to an increased concern over cost, nickel has assumed a position as a major candidate for solar cell metallization. It is shown that sintering can improve the integrity of the nickel-silicon bond. Evidence that the nickel-silicon contact can survive moderate environmental stress is presented.
Sinterless contacts to shallow junction InP solar cells
In the past, the achievement of good electrical contact to InP has inevitably been accompanied by mechanical degradation of the InP itself. Most contact systems require heat treatment after metal deposition that results in the dissolution of substantial amounts of InP into the metallization. Devices such as the solar cell, where shallow junctions are the rule, can be severely degraded if the damage to the semiconductor substrate is not precisely controlled. Two contact systems are described that provide low contact resistance to InP solar cells that do not require subjecting the current carrying metallization to a post deposition sintering process. It is shown that these two systems, one nickel based and the other silver based, provide contact resistivity values in the low 10(exp -6) ohm sq cm range, as fabricated, without the need for sintering.
Development of economical improved thick film solar cell contact
Materials were surveyed to provide candidates for an all metal electrode paste system. These consisted of a major constituent metal powder, a low melting metal powder suitable for a liquid phase sintering medium, and a powder material suitable as an etchant for silicon dioxide at sintering temperatures. By means of thermal gravimetric analysis a suitable binder was identified for low temperature fired inks. The all metal ink concept was first demonstrated with the silver system to avoid the problems of limited process windows encountered with base metal systems. A number of solid materials capable of selectively etching silicon dioxide at modest temperatures were identified. A paste with silver fluoride was screened onto N-type silicon with 5 ohm cm resistivity. The resulting contact pads had excellent adhesion but were not electrically ohmic. Metallurgically, these contacts have equal or better grain structure as commercial inks fired at the same temperatures.
Ultrafast Reactive Laser Sintering of Highly Conductive Garnet-Type LLZTO Solid Electrolytes
Rapid and scalable fabrication of garnet-type solid electrolytes remains a major challenge for the practical deployment of lithium metal batteries. Here, we report reactive laser sintering (RLS) as an ultrafast and potentially scalable strategy for fabricating garnet-type Li 6.4 La 3 Zr 1.4 Ta 0.6 O 12 (LLZTO) solid electrolytes. RLS of LLZTO enables simultaneous reaction and densification, achieving ∼95% relative density while minimizing lithium loss and suppressing secondary phase formation. Compared to conventional furnace sintering, RLS promotes enhanced grain growth and improved densification, leading to improved ionic conductivity (0.36 ± 0.08 mS cm −1 ) while maintaining comparable activation energies for Li + transport. Structural characterization by X-ray diffraction (XRD), Raman spectroscopy, and solid-state 6 Li/ 7 Li NMR confirms the formation of cubic garnet LLZTO with homogeneous microscale elemental distribution. In addition, nanoindentation measurements demonstrate that RLS preserves the mechanical properties of the garnet framework despite ultrafast localized thermal processing. By integrating simultaneous reaction and densification with tunable microstructural control, reactive laser sintering provides a promising manufacturing pathway for high-performance garnet solid electrolytes toward next-generation solid-state batteries.
Dislocation generation during early stage sintering.
Discussion of the effects of capillarity-induced stresses on dislocations during early stage sintering. A special version of Hirth's (1963) theoretical calculation procedures modified to describe dislocation nucleation on planes meeting the sintering body's neck surface obliquely is shown to predict plastic flow at stress levels know to exist between micron size metal particles in the early stages of sintering.
Low resistance silver contacts to indium phosphide - Electrical and metallurgical considerations
The electrical and metallurgical behavior of the Ag-InP contact system has been investigated. Specific contact resistivity (Rc) values in the low 10 exp -6 Ohm sq cm range are readily achieved on n-InP (Si: 1.7 x 10 exp 18/cu cm) after sintering at 400 C for several minutes. The low Rc values, however, are shown to be accompanied by dissolution of InP into the metallization, resulting in device degradation. An analysis of the sinter-induced metallurgical interactions shows this system to be similar to the well-characterized Au-InP system, albeit with fundamental differences. The similarities include the dissociative diffusion of In, the reaction-suppressing effect of SiO2 capping, and especially, the formation of a phosphide layer at the metal-InP interface. The low post-sinter Rc values in the Ag-InP system may be due to the presence of a AgP2 layer at the metal-InP interface; low values of Rc can be achieved without incurring device degrading metallurgical interactions by introducing a thin AgP2 layer between the InP and the current carrying metallization.
Composite fiber structures for catalysts and electrodes
We have recently envisioned a process wherein fibers of various metals in the 0.5 to 15 micron diameter range are slurried in concert with cellulose fibers and various other materials in the form of particulates and/or fibers. The resulting slurry is cast via a wet-lay process into a sheet and dried to produce a free-standing sheet of 'composite paper.' When the 'preform' sheet is sintered in hydrogen, the bulk of the cellulose is removed with the secondary fibers and/or particulates being entrapped by the sinter-locked network provided by the metal fibers. The resulting material is unique, in that it allows the intimate contacting and combination of heretofore mutually exclusive materials and properties. Moreover, due to the ease of paper manufacture and processing, the resulting materials are relatively inexpensive and can be fabricated into a wide range of three-dimensional structures. Also, because cellulose is both a binder and a pore-former, structures combining high levels of active surface area and high void volume (i.e., low pressure drop) can be prepared as freestanding flow through monoliths.
High temperature resistant cermet and ceramic compositions
High temperature oxidation resistance, high hardness and high abrasion and wear resistance are properties of cermet compositions particularly to provide high temperature resistant refractory coatings on metal substrates, for use as electrical insulation seals for thermionic converters. The compositions comprise a sintered body of particles of a high temperature resistant metal or metal alloy, preferably molybdenum or tungsten particles, dispersed in and bonded to a solid solution formed of aluminum oxide and silicon nitride, and particularly a ternary solid solution formed of a mixture of aluminum oxide, silicon nitride and aluminum nitride. Ceramic compositions comprising a sintered solid solution of aluminum oxide, silicon nitride and aluminum nitride are also described.
Array Automated Assembly Task for the Low Cost Solar Array Project, Phase 2
Using silk screened evaporated and sputtered Al as the metal source, the formation of Al back surface fields was studied. The most satisfactory results were those obtained with the sputtered A1 and in which open circuit voltages (V sub oc) of 0.585 v (12 ohm cm FZ silicon) were achieved. The ultrasonic interconnect process is discussed. The process is shown to be satisfactory, but increased pull-strength may be obtained if some form of sintering is carried out on the metallized contacts. Plasma etching is shown to be feasible as a replacement for wet chemical cleaning prior to diffusion. Initial results on cells prepared by using electroless Pd/Ni plus either electroplated Ag or Cu show slightly poor performance than cells with the baseline evaporated Ti/Pd/Ag system. A mask designed for the 1.6 x 7.0 cm and 2.0 x 7.0 cm cells is described. This mask has a lower area coverage and total lower resistive loss than the previous mask design. It is also shown that the cell width should not exceed 2.0 - 3.0 cm for optimum efficiency.