“…This phenomenon can be attributed to a densification of the silica glass network structure. Similar features are observed in the Raman spectra by Perriot et al (2006) in indentation-densified amorphous silica and by Romeis et al (2015) in compression-densified vitreous silica spheres. Previously, compression-induced densification of silica glass was observed by Tomozawa et al (1998) in uniaxial compression experiments and infrared spectroscopy measurements and by Mochizuki and Kawai (1972) in pressure-densified vitreous silica.…”
Section: Workflow For In Situ Tensile Testing Of Silica Glass Membransupporting
confidence: 78%
“…Figure 2 exemplarily shows the results from Raman spectroscopy, while in general good data reproducibility was given. The non-irradiated silica glass membranes exhibit typical Raman spectra with well-known characteristics of vitreous silica on micro- (Perriot et al, 2006) and nanoscale Romeis et al, 2015). The intense band at 440 cm −1 occurs due to stretching of bridging oxygen atoms between two Si atoms.…”
Section: Workflow For In Situ Tensile Testing Of Silica Glass Membranmentioning
The mechanical behavior of glasses in the micro-and nanometer regime increasingly gains importance in nowadays modern technology. However, suitable small-scale preparation and mechanical testing approaches for a reliable assessment of the mechanical properties of glasses still remain a big challenge. In the present work, a novel approach for site-specific preparation and quantitative in situ tensile testing of thin silica glass membranes in the transmission electron microscope (TEM) is presented. Thereby, advanced focused ion beam techniques are used for the preparation of nanoscale dog bone-shaped silica glass specimens suitable for in situ tensile testing. Small amounts of gallium are detected on the surface of the membranes resulting from redeposition effects during the focused ion beam preparation procedure. Possible structural changes of silica glass upon irradiation with electrons and gallium ions are investigated by controlled irradiation experiments, followed by a structural analysis using Raman spectroscopy. While moderate electron beam irradiation does not alter the structure of silica glass, ion beam irradiation results in minor densification of the silica glass membranes. In situ tensile testing of membranes under electron beam irradiation results in distinctive elongations without fracture confirming the phenomenon of superplasticity. In contrast, in situ tensile testing in the absence of the electron beam reveals an elastic/plastic deformation behavior and finally leads to fracture of the membranes. The Young's moduli of the glass membranes pulled at beam-off conditions in the TEM are comparable with values known for bulk fused silica, while the tensile strength is in the range of values reported for silica glass fibers with comparable dimensions. The impact of electron beam irradiation on the mechanical properties of silica glass membranes is further discussed. The results of the present work open new avenues for dedicated preparation and nanomechanical characterization of silica glass and further contribute to a fundamental understanding of the mechanical behavior of such glasses when being scaled down to the nanometer regime.
“…This phenomenon can be attributed to a densification of the silica glass network structure. Similar features are observed in the Raman spectra by Perriot et al (2006) in indentation-densified amorphous silica and by Romeis et al (2015) in compression-densified vitreous silica spheres. Previously, compression-induced densification of silica glass was observed by Tomozawa et al (1998) in uniaxial compression experiments and infrared spectroscopy measurements and by Mochizuki and Kawai (1972) in pressure-densified vitreous silica.…”
Section: Workflow For In Situ Tensile Testing Of Silica Glass Membransupporting
confidence: 78%
“…Figure 2 exemplarily shows the results from Raman spectroscopy, while in general good data reproducibility was given. The non-irradiated silica glass membranes exhibit typical Raman spectra with well-known characteristics of vitreous silica on micro- (Perriot et al, 2006) and nanoscale Romeis et al, 2015). The intense band at 440 cm −1 occurs due to stretching of bridging oxygen atoms between two Si atoms.…”
Section: Workflow For In Situ Tensile Testing Of Silica Glass Membranmentioning
The mechanical behavior of glasses in the micro-and nanometer regime increasingly gains importance in nowadays modern technology. However, suitable small-scale preparation and mechanical testing approaches for a reliable assessment of the mechanical properties of glasses still remain a big challenge. In the present work, a novel approach for site-specific preparation and quantitative in situ tensile testing of thin silica glass membranes in the transmission electron microscope (TEM) is presented. Thereby, advanced focused ion beam techniques are used for the preparation of nanoscale dog bone-shaped silica glass specimens suitable for in situ tensile testing. Small amounts of gallium are detected on the surface of the membranes resulting from redeposition effects during the focused ion beam preparation procedure. Possible structural changes of silica glass upon irradiation with electrons and gallium ions are investigated by controlled irradiation experiments, followed by a structural analysis using Raman spectroscopy. While moderate electron beam irradiation does not alter the structure of silica glass, ion beam irradiation results in minor densification of the silica glass membranes. In situ tensile testing of membranes under electron beam irradiation results in distinctive elongations without fracture confirming the phenomenon of superplasticity. In contrast, in situ tensile testing in the absence of the electron beam reveals an elastic/plastic deformation behavior and finally leads to fracture of the membranes. The Young's moduli of the glass membranes pulled at beam-off conditions in the TEM are comparable with values known for bulk fused silica, while the tensile strength is in the range of values reported for silica glass fibers with comparable dimensions. The impact of electron beam irradiation on the mechanical properties of silica glass membranes is further discussed. The results of the present work open new avenues for dedicated preparation and nanomechanical characterization of silica glass and further contribute to a fundamental understanding of the mechanical behavior of such glasses when being scaled down to the nanometer regime.
“…For all contacts a 0.1 friction coefficient was used with a Penalty formulation. We have calculated the flat punch compression of a sphere to emulate available data (Romeis et al (2015)). Based on the experimental results, we plot the maximum reaction force for a 0.927 micron punch penetration on a 4.17 micron silica sphere in Fig.…”
Section: Calibration Proceduresmentioning
confidence: 99%
“…Good agreement is found with the experiments, further demonstrating that the form of the yield function is reasonable and the parameter values adequate. (Field et al (2003); Iwashita and Swain (2002)); b) Nanosphere compression (Romeis et al (2015)).…”
“…Moreover, it was argued that by using Equation a higher experimental reproducibility is achieved compared to using the positions of a single defect line alone . In addition to fused silica, this method was successfully applied to soda lime silicate and other glass systems …”
Inelastic deformation of anomalous glasses manifests in shear flow and densification of the glass network; the deformation behavior during indentation testing is linked strongly to both processes. In this paper, the indentation densification field of fused silica is investigated using depth‐resolved Raman spectroscopy and finite element simulations. Through affecting the size of the indent, the normal load and the Raman laser spot size determine the spatial sampling resolution, leading to a certain degree of structural averaging. For appropriate combinations of normal load (indent size) and laser spot diameter, a maximum densification of 18.4% was found at the indent center. The indentation behavior was modeled by extended Drucker‐Prager‐Cap (DPC) plasticity, assuming a sigmoidal hardening behavior of fused silica with a densification saturation of 21%. This procedure significantly improved the reproduction of the experimental densification field, yielding a maximum densification of 18.2% directly below the indenter tip. The degree of densification was found to be strongly linked to the hydrostatic pressure limit below the indenter in accordance to Johnson's expanding cavity model (J. Mech. Phys. Solids, 18 (1970) 115). Based on the good overlap between FEA and Raman, an alternative way to extract the empirical correlation factor m, which scales structural densification to Raman spectroscopic observations, is obtained. This approach does not require the use of intensive hydrostatic compaction experiments.
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