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185 cracks were initiated in a soda-lime-silica glass by Vickers indentation and grown under controlled dry nitrogen atmosphere. Direct observation of subcritical crack growth (SCCG) upon indentation was performed using a video camera with an image acquisition rate of 3 ms. The results show that the validity of K(c) relations used to determine the indentation fracture toughness from a single imprint is questionable. It seems that correlation of crack length to stress intensity necessitate the use of statistical significant data of multiple crack events.
Um das Risswachstum in Gläsern zu untersuchen, sind in einer Glovebox 185 Risse ausgehen von Vickers-Eindrücken in Kalk-Natron-Glas initiiert und gewachsen. Die direkte Beobachtung des unterkritischen Risswachstums erfolgte mit einer Hochgeschwindigkeitskamera. Die Ergebnisse zeigen, dass die statistische Auswertung vieler radialer Risse von multiplen Rissevents notwendig ist, um eine Korrelation zum Spannungsintensitätsfaktor ziehen zu können.
Water has a strong impact on the viscosity and the transition temperature of oxide glasses. It acts as a fluxing agent, reducing viscosity particularly in the glass transition range, and by that flattening the viscosity-temperature curve and decreasing the fragility of hydrous glass melts. This general behavior is found for silicate and borate as well as in borosilicate compositions. However, there is still a lack of data with respect to hydrous phosphate glasses. Here, we study the influence of structural water on the viscosity of Li2O-MgO-(Al2O3-)P2O5 glasses. The glasses were synthesized in an internally heated pressure vessel (IHPV) at a pressure of 0.5 GPa. The selected pressure allows for the synthesis of glass specimens with water contents of several wt.%. The viscosity measurements were carried out in the glass transition range, i.e. log η ≈ 10-13 (η in Pa s), using a sphere penetration viscometer. The measured data agree with glass transition temperatures measured by differential thermo analysis. First results further suggest that the fragility of the analyzed phosphates decreases with increasing water content.
Statistical analysis of Vickers induced subcritical crack growth in soda-lime silicate glasses
(2018)
Studies on Vickers induced subcritical crack growth are controversially discussed since the stresses that drive the crack growth are distributed three dimensionally within the material and cannot be retraced by available methods. Hence, empirical approaches are used to calculate mechanical material parameters such as the stress intensity factor KI. However, the results of these approaches show large deviations from those measured by standardized techniques such as double cantilever beam (DCB) or double cleavage drilled compression (DCDC). Yet, small specimen sizes and low specimen quantities can prevent the execution of DCB and DCDC measurements. Here we present an approach that is based on a statistical analysis of Vickers induced radial cracks. For this purpose more than 150 single radial cracks were analyzed. The cracks were generated in a commercial soda-lime silicate glass. The experiments were performed in a glovebox purged with dry nitrogen gas to minimize the influence of atmospheric water on crack growth. The temporally resolved evolution of the radial cracks was monitored in-situ using an inverted microscope equipped with a camera system directly below the Vickers indenter. An automated image analysis software was used to determine the crack length over time. The data show that the crack propagation and thereby the crack velocities are not uniformly but statistically distributed. These findings allow, using the statistical mean value of the distributions in combination with DCB data, a precise formulation of KI for each measured crack length.
The presence of water in the surrounding atmosphere of a propagating crack has a major influence on the subcritical crack growth. While these external phenomena are well understood, there is still a lack of knowledge on the influence of structurally bound water on crack propagation. Thus, our recent study aims on the analysis of crack propagation in water bearing soda-lime silicate glasses with up to 8 wt.% water. The samples were synthesized in an internally heated pressure vessel at 0.5 GPa. Since this preparation route limits the sample sizes, standard test geometries allowing for the determination of stress intensity factors, such as double cantilever beam, are not feasible. Thus, radial cracks in the hydrous glasses were initiated by Vickers indentation and crack growth was simultaneously captured with a camera system. An automated image analysis algorithm was used for the analysis of the crack length of each single video frame. To minimize influences by atmospheric water, all experiments were conducted in a glovebox purged with dry N2. About 150 cracks per glass composition were analyzed to provide statistical significance of the Vickers-induced SCCG. The results show that structurally bound water has a major influence on SCCG by means of crack lengths, growth rates and time of crack initiation.