ABSTRACT
High-throughput combinatorial investigations are transforming materials discovery, phase diagram development, and processing optimization. Thin-film deposition techniques are frequently used to fabricate sample libraries employed in these studies. Various adaptations of well-known thin-film chemical vapor deposition (CVD) and physical vapor deposition (PVD) techniques utilized for the synthesis of inorganic combinatorial thin-film materials libraries are reviewed, with novel processing approaches being highlighted. Methods for developing gradients in composition of other film properties are described. Issues and considerations specific to thin-film processing of combinatorial materials libraries are discussed, with some emphasis on catalytic applications.
Subject(s)
Combinatorial Chemistry Techniques , High-Throughput Screening Assays , Combinatorial Chemistry Techniques/instrumentation , High-Throughput Screening Assays/instrumentation , Optical DevicesABSTRACT
A combinatorial synthesis and high-throughput screening process was developed for the investigation of potential oxygen reduction reaction (ORR) and oxygen evolution reaction (OER) catalysts for use as Li-air battery cathode materials. Libraries of discrete ternary metal alloy compositions were deposited via thin-film sputtering. The samples were electrochemically tested in parallel using cyclic voltammetry in O2-saturated KOH electrolyte. Compositions were ranked by ORR and OER onset potentials with respect to an internal Pt reference. Results from the Pt-Mn-Co, Cr-Mn-Co, Pd-Mn-Co, and Pd-Mn-Ru systems are reported. Many alloy compositions showed marked improvement in catalytic activity compared to pure Pt. Among the systems considered, Pt12Mn44Co44, Pd43Co57 and Pd36Mn28Ru36 in particular exhibited lower overpotentials for oxygen reactions, which occur at the cathode in Li-air batteries.
Subject(s)
Combinatorial Chemistry Techniques/methods , Electric Power Supplies , Lithium/chemistry , Air , Alloys , Catalysis , Electrochemical Techniques , Hydroxides/chemistry , Metals/chemistry , Oxidation-Reduction , Potassium Compounds/chemistry , X-Ray DiffractionABSTRACT
Bulk processing of porous silicon nanoparticles (nSi) of 50-300 nm size and surface area of 25-230 m(2)/g has been developed using a combustion synthesis method. nSi exhibits consistent photoresponse to AM 1.5 simulated solar excitation. In confirmation of photoactivity, the films of nSi exhibit prompt bleaching following femtosecond laser pulse excitation resulting from the photoinduced charge separation. Photocurrent generation observed upon AM 1.5 excitation of these films in a photoelectrochemical cell shows strong dependence on the thickness of the intrinsic silica shell that encompasses the nanoparticles and hinders interparticle electron transfer.
ABSTRACT
We describe development of a relatively simple, rapid route to produce combinatorial compositional oxide powder libraries by autopipetting of liquid precursors. This partitioning approach should apply equally well to any low viscosity, liquid precursors for the synthesis of oxide powders. A commercial autopipet is modified by fitting a plastic "mask" assembly beneath the pipet array in order to partition and direct liquids into crucibles. A series of 10 mixtures from two precursor solutions can be produced quickly. After they are dispensed, the liquid mixtures are dried in the crucibles and reacted at elevated temperatures to produce oxide powders. In the present work, the viability of the pipetting process is demonstrated by using a polymerizable complex powder synthesis method to produce (1-x) LaAlO(3) - x SrTiO(3) powders. For this system, a reaction at 900 degrees C for 2 h in air was sufficient to yield solid solutions in this system. X-ray powder diffraction was used to determine the pseudocubic unit cell lattice parameter. The linear change of lattice constant with composition confirms the compositional accuracy of the partitioning.
