Journal of the American Ceramic Society, Vol.84, No.4, 795-800, 2001
Dye impregnation method for revealing machining crack geometry
The palladium nitrate dye penetrant method for revealing surface microcracks was investigated and applied to display the geometry of machining cracks in silicon nitride flexure test specimens. This method used elemental mapping with an electron probe microanalyzer to detect the presence of the dye and, thereby, display the crack geometry. A previously used bending method and a method developed in this study in which the specimen surface is exposed to the dye under pressure were used to facilitate dye penetration. Prior to applying the method to study machining cracks, carefully controlled Knoop indentation cracks introduced into flexure specimens were used to verify penetration of the dye to the crack tip. During these experiments it was found that the palladium nitrate dye resulted in a reduction in flexure strength, which, on further study, was attributed to the dilute nitric acid solution used to formulate the dye. Exposure to carbon tetrafluoride plasma etching prior to applying the pressurized dye method also resulted in a detectable decrease in flexure strength. Although there was clear evidence that exposure to dye and plasma etching resulted in a small but measurable decrease in flexure strength for the silicon nitride material studied, there was no detectable change in observed crack geometry. The reduction in flexure strength was apparently caused by a decrease in resistance to initiate crack propagation. It was concluded that the palladium nitrate dye method is an accurate and useful means for determining the geometry of small, otherwise difficult to observe surface microcracks, Nevertheless, caution should be exercised with the use of this method during strength measurements. When applied to machining cracks, the complex nature of these shallow, elongated, sometimes joining cracks was unambiguously revealed.