Quantitative determination of ZrC in new ceramic materials by Fourier transform infrared spectroscopy

Abstract Zirconium carbide-based biomorphic ceramics have been manufactured by vacuum infiltration of zirconium-oxychloride (ZrOCl2·8H2O) sol into natural wood. After vacuum-assisted infiltration, the specimens were dried in air and pyrolysed at 800 °C in Ar-atmosphere. The infiltration and drying process were repeated up to four times. Finally, the specimens were hold at 1550 °C in a vacuum furnace to form ZrC. The results of the process of synthesis have been studied using scanning electron microscopy (SEM). For evaluating the yield of the synthesis, a new method by Fourier transform infrared spectrometry (FTIR) has been developed for the direct determination of ZrC by absorbance measurements in KBr pellets. The procedure was based on the use of the ratio between the absorbance of the characteristic band of zirconium carbide and those of an oxalate internal standard added to samples. A multivariate calibration strategy based on inverse least squares and the standard addition approach was employed for quantification. The results obtained for all ZrC-ceramics studied were satisfactorily compared with those obtained by X-ray diffractometry (XRD). The proposed method was also applied to the analysis of synthetic samples prepared by mixing pyrolyzed wood with ZrC, the results indicated good recovery in all instances.