Ceramic oxide materials, analysis

Typical characterization of the thermal conversion process for a given molecular precursor involves the use of thermogravimetric analysis (TGA) to obtain ceramic yields, and solution NMR spectroscopy to identify soluble decomposition products. Analyses of the volatile species given off during solid phase decompositions have also been employed. The thermal conversions of complexes containing M - 0Si(0 Bu)3 and M - 02P(0 Bu)2 moieties invariably proceed via ehmination of isobutylene and the formation of M - O - Si - OH and M - O - P - OH linkages that immediately imdergo condensation processes (via ehmination of H2O), with subsequent formation of insoluble multi-component oxide materials. For example, thermolysis of Zr[OSi(O Bu)3]4 in toluene at 413 K results in ehmination of 12 equiv of isobutylene and formation of a transparent gel [67,68]. 

Hydroxycarboxylic acids, which include citric acid, malic acid, lactic acid, etc., are benign to the environment and very convenient for the solution processing. Moreover, since these reagents can form stable complexes with other cations, they rarely yield a precipitate. For several complexes single crystals of well-defined composition suitable for the X-ray structural analysis were isolated. Thus, these water-soluble titanium complexes of hydroxycarboxylic acids are promising precursors for the synthesis of ceramics from an aqueous solution and their industrial utilization is expected in the future. In this chapter we decribe the method of synthesis, structural analysis, and stability of these complexes. The examples of multicomponent oxide materials preparation using these compounds are presented. 

Chem. Descrip. Hollow ceramic microspheres Chem. Analysis Shell material SiOs (59 /o), AIA (38%), TIQ2 (1.7%), iron oxides (0.5 /o)... 

Chemical analysis of niobium oxide indicated that the purity of the final product depends strongly on the purity of the initial solution. Account should be taken of about 0.02-0.03% wt. cationic impurities, introduced due to interactions with metal parts of the equipment. The main added impurities are Fe, Ni, Cr, which originate mostly from the stainless steel filter. The purity of the final product can be significantly increased by using a filter made of niobium or other appropriate material. Nevertheless, the material obtained using a stainless steel filter is sufficient for use in ceramic applications or as an initial material for carbide manufacture. 

The first useful organosilicon preceramic polymer, a silicon carbide fiber precursor, was developed by S. Yajima and his coworkers at Tohoku University in Japan [5]. As might be expected on the basis of the 2 C/l Si ratio of the (CH3)2SiCl2 starting material used in this process, the ceramic fibers contain free carbon as well as silicon carbide. A typical analysis [5] showed a composition 1 SiC/0.78 C/0.22 Si02- (The latter is introduced in the oxidative cure step of the polycarbosilane fiber). 

Mossbauer spectroscopy is a selective tool for the quantitative analysis and spe-ciation of a very limited number of elements. It has been mainly used to study iron compounds—e.g., ceramics, as it gives valuable information about iron-bearing oxide and silicate minerals. This technique has been applied to the identification of the provenance of clay and used raw materials—the manufacturing method employed in pottery and, to a lesser extent, to the characterization of pigments and weathering crusts formed on stone monuments [23]. 

And now another important question is Should these Venus sculptures be classed as ceramic materials Initial analyses proved that they were made of silicon-containing ash and mammoth bone and possibly also mammoth fat, but no aluminium oxide or potassium oxide - which are always present in clay - were found. A later analysis of the Venus of Vestonice led to the concusion that a mixture of mammoth fat and bone, mixed with bone ash and local loess had been used but still no traces of potassium nor of aluminium. In the eighties the Venus was examined using more sophisticated equipment and the result was no bone or other organic components and no stone fragments. In the period 1955-1965 some researchers concluded that the animal statues of Dolni Vestonice were made of clay, and they called this terra cotta which means burned soil . Present studies indicate that the loess of Dolni Vestonice was used as raw material for the animal figurines. 

Recognizing the applicability of XRD to occupational health chemistry, Lennox and Leroux (1) suggested a number of chemical species which would be suitable for XRD analysis arsenic trioxide, beryllium oxide, mica, vanadium oxides, calcium fluoride in ceramic materials, as well as a number of organics such as DDT, lindane and chlordane. Unfortunately, the general application of XRD to the quantitation of industrial hygiene samples has not been realized and the majority of these analyses are restricted to free silica and to a lesser extent asbestos and talc. 

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