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Quantitative Analysis of Polymorphic Mixes of Zirconia by X‐ray Diffraction
Author(s) -
SCHMID H. K.
Publication year - 1987
Publication title -
journal of the american ceramic society
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.9
H-Index - 196
eISSN - 1551-2916
pISSN - 0002-7820
DOI - 10.1111/j.1151-2916.1987.tb05009.x
Subject(s) - calibration curve , monoclinic crystal system , diffraction , materials science , tetragonal crystal system , analytical chemistry (journal) , cubic zirconia , ternary operation , powder diffraction , intensity (physics) , x ray crystallography , reflection (computer programming) , crystallography , chemistry , crystal structure , optics , ceramic , chromatography , metallurgy , detection limit , programming language , physics , computer science
Nonlinear calibration curves of weight fraction vs integrated intensity ratio arc obtained for polymorphic mixtures of ZrO 2 by means of powder X‐ray diffraction. The (C + M) and (T + M) ZrO 2 systems are analyzed using the {111} reflections. Intensity ratios in mixtures prepared with an ultrafine m ‐ZrO 2 powder agree well with theoretical values. The observed nonlinearity of the intensity‐concentration curve is explicable from the differences in reflecting power of corresponding reflections in the three polymorphs. Considerable deviations from theoretical intensity ratios are observed in mixtures prepared with coarser commercially available m ‐ZrO 2 powders. This effect is attributed to an anomalously high absorption behavior of those monoclinic materials and can be suppressed by quenching in liquid nitrogen, which is believed to cause the particles to shatter. The (C + T) ZrO 2 system is analyzed using the {200} reflections rather than the more usual high‐angle reflections and the derived nonlinear calibration curve agrees well with theoretical prediction. In the ternary system (C + T + M) ZrO 2 the presence of tetragonal phase can be confirmed by microphotometric tracing of the {111} and {200} reflection profiles on Guinier photographs, but in this case a quantitative analysis would be difficult.