High Throughput Synthesis of Pigments by Solution Deposition
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High Throughput Synthesis of Pigments by Solution Deposition
Stuart J. Henderson*, Andrew L. Hector and Mark T. Weller. School of Chemistry, University of Southampton, Highfield, Southampton, SO17 1BJ, UK. ABSTRACT Combinatorial and high throughput methods have been utilised in the pharmaceutical industry for many years. The process involves the simultaneous synthesis of libraries containing thousands of compounds, which can then be screened for desirable properties. More recently the concepts of parallel synthesis and high-throughput screening have emerged as effective strategies in the search for novel inorganic materials. We report the development of high throughput methods, which have been used for the synthesis and preliminary characterisation of ceramic oxide pigments on an alumina substrate. This methodology has been utilised to prepare compounds with the spinel structure in the series Cu1-xZnxAl2-yCryO4 (0# x #1, 0# y #2) at a range of temperatures. The materials are analysed by rapid sequential X-ray diffraction and a simple colour measurement technique. The optical properties across the quaternary landscape can therefore be mapped as a function of composition, structure and annealing temperature. INTRODUCTION The application of high throughput methods for the synthesis and screening of inorganic materials is an area of growing interest [1,2]. The ability to rapidly assess the properties of large numbers of discrete compounds prepared using small quantities of reagents make these techniques attractive for both industrial and academic research. Much of the literature focuses on the preparation of thin film arrays by vapour deposition [3,4]. However, such samples may not give a true indication of the material’s properties when prepared as a bulk powder. Libraries of powdered catalysts and phosphor materials prepared from solutions have been shown to be an effective lower cost route to novel inorganic materials [5,6]. High-throughput methods for materials development presents different challenges to those faced in the pharmaceutical field. The properties for which the material needs to be screened are much more varied and are often unique for each system. It is often the case that physical treatments are very significant in determining which phase forms. We present the development of a high throughput method for preparing arrays of pigments from solutions, which can subsequently be screened for their colour properties. To assess the validity of the technique we have applied it to pigment materials for which the optical and structural properties are already established. Compounds with the spinel structure (AB2O4) nominally varying Cu/Zn on the A site and Al/Cr on the B site have previously been investigated as catalysts for the decomposition of ammonium nitrate [7]. The end members in this series have also been investigated for pigment applications (ZnCr2O4 brown, CuCr2O4 black, CuAl2O4 red-brown, ZnAl2O4 white [8,9]). This quaternary system was therefore suitable for the purpose of developing the hi
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