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Stable crack growth was measured for nominal dry and water-bearing (6 wt%) soda-lime silicate glasses in double cantilever beam geometry and combined with DMA studies on the effects of dissolved water on internal friction and glass transition, respectively. In vacuum, a decreased slope of logarithmic crack growth velocity versus stress intensity factor is evident for the hydrous glass in line with an increase of b-relaxation intensity indicating more energy Dissipation during fracture. Further, inert crack growth in hydrous glass is found to be divided into sections of different slope, which indicates different water related crack propagation mechanism. In ambient air, a largely extended region II is observed for the hydrous glass, which indicates that crack growth is more sensitive to ambient water.
The neutron time-of-flight spectrometer NEAT has a long history of successful applications and is best suited to probe dynamic phenomena directly in the large time domain 10(-14) - 10(-10) s and on the length scale ranging from 0.05 to up to about 5 nm. To address user community needs for more powerful instrumental capabilities, a concept of the full upgrade of NEAT has been proposed. The upgrade started in 2010 after a rigorous internal and external selection process and resulted in 300-fold neutron count rate increase compared to NEAT01995. Combined with new instrumental and sample environmental capabilities the upgrade allows NEAT to maintain itself at the best world class level and provide an outstanding experimental tool for a broad range of scientific applications. The advanced features of the new instrument include an integrated guide-chopper system that delivers neutrons with flexible beam properties: either highly homogeneous beam with low divergence suitable for single crystals studies or "hot-spot" neutron distribution serving best small samples. Substantial increase of the detector angle coverage is achieved by using 416 He-3 position sensitive detectors. Placed at 3m from the sample, the detectors cover 20m(2) area and are equipped with modern electronics and DAQ using event recording techniques. The installation of hardware has been completed in June 2016 and on January 23, 2017 NEAT has welcomed its first regular users who took advantage of the high counting rate, broad available range of incoming neutron wavelengths and high flexibility of NEAT. Here we present details of NEAT upgrade, measured instrument characteristics and show first experimental results.
To explore the impact of ambient and structural water on static fatigue, the initiation and growth of 3279 Vickers induced median radial cracks were automatically recorded and analyzed. We find that humidity is more efficient in initiating cracks and promoting their growth than water, which is dissolved in the glass structure. In particular for slow crack growth (< 3x10-6 m s-1), tests in dry nitrogen showed a considerable decrease in the crack growth exponent with increasing water content of the glasses. On the other hand, if tests were performed in humid air, the crack growth exponent was independent of the water content of the hydrous glasses, while stress intensity decreased slightly. These observations indicate that water promotes the processes at the crack-tip regardless of its origin. However, ambient water is more efficient.
Due to the stochastic nature of crack nucleation by Vickers indentation, a statistical analysis of propagation rates of 185 radial cracks was performed. Crack growth was observed directly using a video camera with high Image acquisition rate. It is found that propagation rates are controlled by the environmental reactions at the crack-tip shortly after their initiation (< 1 s). Calibration of the stress intensity KI showed that the residual stress factor χ and the exponent n of the equation KI==χPc−n (with P==load and c==crack length) are broadly distributed among the 185 analyzed cracks, ranging from 10−16 to 104 and from 0.1 to 5, respectively. For the most frequent crack, the equation KI==0.052Pc−1.47 holds. The results show that correlations of indentation-induced crack length to stress intensity necessitate the use of statistical significant data that are calibrated by the environmental reactions at the crack-tip.
The effect of structural water on density, elastic constants and microhardness of water-bearing soda-lime-silica glasses of up to 21.5 mol% total water is studied. It is found that the Poisson ratio and the water content are positively correlated, while density and the elastic moduli decrease with increasing water content. Vickers hardness decreases by approximately 27% from the dry to the most hydrous glass. For water fractions <3 mol%, the dependencies are non-linear reflecting the non-linear change in the concentrations of OH and H2O molecules dissolved, whereas for water fractions >3 mol% linear dependencies are found. To distinguish the effect of structural water and environmental water, indentations were performed in toluene, nitrogen gas and air. Timedependent softening was evident for testing dry glasses in humid atmospheres as well as for tests of hydrous glasses in dry atmospheres. This indicates that the response times of dissolved water species are effectively equal in both scenarios.
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.
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.