Toward revealing atomic deformation mechanics in lithium disilicate and β-quartz containing glass-ceramics

The mechanics of glass-ceramics subjected to sharp contact or other loading conditions remain elusive, even after being commercialized in many industrial applications. We present work herein to reveal atomic details of such deformations that are otherwise extremely difficult to probe experimentally for a lithium disilicate (LS2) and β-quartz containing glass-ceramics via molecular dynamics simulations. Specifically, the materials are comprised of LS2 and β-quartz nanocrystals in a residual glass matrix. Regardless of the deformation mechanism, whether it be nanoindentation or crack propagation for samples with pre-existing flaws, we observe that the LS2 nanocrystal itself undergoes substantial deformation, either by activating dislocations, forming an amorphization zone, or by initiating microcracks at glass-crystal interfaces or weak crystallographic planes. In contrast, the β-quartz nanocrystal is not easily deformed and remains almost intact with minimal plastic deformation, thereby forcing shear flow and crack propagation pathways to predominately occur in the residual glass and/or at interfaces. The dramatic difference between the crystalline phases also manifests itself in the deformation mode of interfaces under pure shear loading, in which shear bands preferably occur at the LS2-glass interfaces, while cavities form at the β-quartz-glass interfaces. These observations significantly advance our understanding of glass-ceramics and pave ways to exploit the understanding for more applications.     

Mechanical Properties of Mica Glass-Ceramics

The mechanical properties of fluorophlogopite mica-based glass-ceramics, such as fracture toughness, flexural strength, and machinability, were investigated. It has been shown that toughening increments in the glass-ceramics occurred by crack deflection and branching by crystals with a high aspect ratio. All the glass-ceramics heat treated at 1000°–1150°C exhibited a higher fracture toughness of 1.2–2.2 MPa-m^1/2 as compared to 0.8 MPa-m^1/2 for the parent glass, and showed average flexural strengths of 140–160 MPa. It has been suggested that ( H/K_Ic )² of the mica glass-ceramic be used to estimate the machinability, because it decreases linearly with machinability.     

High-Temperature Failure of an Alumina-Silicon Carbide Composite under Cyclic loads: Mechanisms of Fatigue Crack-Tip Damage

Experimental results are presented on the mechanisms of tensile cyclic fatigue crack growth in an A1₂0₃-33-vol%-SiC-whisker composite at 1400°C. The ceramic composite exhibits subcritical fatigue crack propagation at stress-intensity-fator values far below the fracture toughness. The fatigue characterized by the stressintensity-factor range, ΔK, and crack propagation rates are found to be strongly sensitive to the mean stress (load ratio) and the frequency of the fatigue cycle. Detailed transmission electron microscopy of the fatigue crack-tip region, in conjunction with optical microscopy, reveals that the principal mechanism of permanent damage ahead of the advancing crack is the nucleation and growth of interfacial flaws. The oxidation of Sic whiskers in the crack-tip region leads to the formation of a silica-glass phase in the 1400°C air environment. The viscous flow of glass causes debonding of the whisker-matrix interface; the nucleation, growth, and coalescence of interfacial cavities aids in developing a diffuse microcrack zone at the fatigue crack tip. The shielding effect and periodic crack branching promoted by the microcracks result in an apparently benefcial fatigue crack-growth resistance in the A1₂0₃—SiC composite, as compared with the unreinforced alumina with a comparable grain size. A comparison of static and cyclic load crack velocities is provided to gain insight into the mechanisms of elevated temperature fatigue in ceramic composites.     

A novel process of preparing glass-ceramics with pseudo-bioclastic texture

Water quenching-induced cracked-glass was used as parent glass to prepare glass-ceramics in this work. The cracked-glass panel was first heat-treated through two-step method, i.e. sintering for 1 h at 860 °C and subsequent crystallization for 1.5 h at 1080 °C, and then naturally cooled down to room temperature to be transformed into glass-ceramics. XRD and SEM observations confirm that the cracked-glass can be used as parent glass to deposit β-wollastonite crystals depending on crack crystallization mechanism. The volume densities, porosities and bending strengths of the glass-ceramics are respectively around 2.7 g/cm³, 0.5% and 40 MPa. As compared with glass-ceramics prepared by conventional glass grain sintering process, the new type of glass-ceramics produced by CGC process shows pseudo-bioclastic texture and has less gas pore flaws, and may therefore become an alternative for materials of architectural decoration.     

Effect of Crystallites on Surface Damage and Fracture Behavior of a Glass-Ceramic

A study was conducted of the effect of crystallization on the fracture toughness, strength, and resistance to surface damage of glass-ceramic materials with a range of microstructures obtained by different heat treatments. The hardness indentation method was used as a quantitative tool to simulate mechanical surface damage. In the uncrystallized glass and in the glass-ceramic heat-treated to result in a uniform fine-grained structure, crack size increased monotonically with indentation load. In contrast, in the glass-ceramics heat-treated to result in a microstructure consisting of larger crystallites (a few micrometers) contained within a fine-grained matrix, a discontinuity in the crack size vs load curve presented evidence for crack-pinning at crack sizes which were a small multiple of the intercrystallite spacing. At the position of crack-pinning, the fracture toughness showed a discontinuous increase with increasing crack size that was attributed to crack deflection. The strength of the glass and fine-grained glass-ceramic measured in biaxial flexure decreased monotonically with indentation load. The strength at low values of indenter load of the glass-ceramic heat-treated to yield the coarser crystallites within the fine-grained matrix was independent of indentation load, indicating stable crack propagation prior to fast fracture. At the higher values of indenter load, the coarse-grained glass-ceramics exhibited a monotonic decrease in strength with increasing indentation load. The results of this study indicate that the strengthening observed on crystallization of a glass can be attributed to a combination of a decrease in flaw size achieved at a given mechanical surface treatment, an increase in fracture toughness, and a modification in the mode of crack propagation.     

Toughening of Li2O-2SiO2 glass-ceramics induced by intriguing deformation behavior of lithium disilicate nanocrystal

We report a toughening mechanism of Li ₂ O-2SiO₂ glass-ceramics induced by intriguing anisotropic deformation behavior of lithium disilicate nanocrystal under tensile loadings using molecular dynamics simulations. The nanocrystal undergoes clear brittle cleavage when loaded in the [010] direction, while exhibiting a first-order deformation-induced transition when loaded in the [100] direction. The transition is exclusively facilitated by local Li–O bond breaking, which spreads to the whole sample under continuous loading. This hierarchical deformation mechanism (exclusive Li–O bond breakage prior to any Si–O bond breakage) enables lithium disilicate nanocrystal bearing large amounts of deformation without breaking. We further demonstrate that the toughness of Li ₂ O-2SiO₂ glass-ceramics can be significantly enhanced by deliberate designs of nanocrystal distributions in glass. The direct observation of this intriguing deformation behavior might inspire new ideas to design tougher lithium disilicate glass-ceramics.     

Cr2 O3、TiO2对高炉渣制备微晶玻璃晶化方式的影响

以包钢高炉渣为主要原料,采用熔融法制备CaO-SiO2-MgO-Al2O3系微晶玻璃,主要通过差热分析方法,并借助于Augis-Bennett方程和Ozawa方程研究了分别添加2%Cr2O3和8%TiO2作晶核剂时基础玻璃的晶化方式.研究结果表明:添加2%Cr2O3作晶核剂时,晶体生长指数均可实现大于3,晶化方式为整体晶化;而添加8%TiO2作晶核剂时,晶体生长指数均不可能大于3,晶化方式为表面晶化.因此,Cr2O3是高炉渣制备透辉石类微晶玻璃适宜的晶核剂成分,可单独用作晶核剂,而TiO2无法使基础玻璃整体晶化,不能单独用作晶核剂.研究结果为利用高炉渣成功研制开发透辉石类微晶玻璃在晶核剂种类选择确定方面提供了理论指导.     

A fractal analysis of crack branching in borosilicate glass

Many fractography techniques involve precise measurements of features on the fracture surface and can be difficult to perform in the field, or rapidly. Macroscopic crack branching observations offer a more robust and forgiving method of analysis, but often are not strongly correlated with standard fractography techniques. In this study, the crack branching patterns of annealed borosilicate glass disks previously fractured in biaxial tension were analyzed using fractal methods and compared with more typical fracture surface measurement techniques. The results confirm that the fractal dimension of macroscopic crack branching (called the Crack Branching Coefficient) increases with increasing failure stress, as has been shown with other brittle materials. In addition, the existence of a threshold stress previously reported was confirmed using new techniques. The findings herein can be used to further increase the fidelity of fractography-based failure analysis of brittle materials.     

玻璃的脆性(四)

综述了裂纹的容忍度与玻璃脆性的关系。对不同品种玻璃的裂纹扩展力也作了阐述。此外,还讨论了应力腐蚀下各种玻璃的裂纹扩展速度和影响裂纹扩展的因素。     

Fracture mechanism of alumina-spinel castables containing ZrO2 by wedge splitting test and digital image correlation technique

To clarify the fracture mechanism of alumina-spinel castables, two kinds of alumina-spinel castables with or without fused zirconia-alumina (FZA) were prepared. The full-field strains and crack propagation process in the region of interest (ROI) of alumina-spinel castables were investigated by wedge splitting test (WST) and digital image correlation (DIC) technique. Fractographic methods were used to analyze the crack propagation path of the castables after the WST. The results indicated that the load-displacement curve of alumina-spinel castables containing FZA exhibits a non-linear fracture, demonstrated typical ductile fracture; while that of alumina-spinel castables without FZA is linear, showed typical brittle fracture. The characteristic length reaches to 258.9 mm in FZA containing castables, more than 4 times that of the castables without FZA. In contrast, castables containing FZA has longer and more tortuous crack propagation path, larger damage zone length, which results in the increase of the dissipated energy. Crack branching can be observed around the main crack in castables containing FZA, meaning that microcracks toughening is the main mechanism for flexibility improvement of the alumina-spinel castables containing FZA, formation of micro-cracks can be attributed to the martensitic transformation of zirconia.     

Investigation of microscale fracture mechanisms in glass–ceramics using peridynamics simulations

Glass–ceramics (GCs), obtained by controlled crystallization of a specially formulated precursor glass, are interesting materials that show great promise in obtaining superior properties compared to those of the precursor glass. Controlled crystallization enables creation of a microstructure with multiple phases which impacts macroscale properties in interesting ways. The present work develops microstructure-scale computational models using the theory of peridynamics to investigate the increase in fracture toughness of GCs compared to traditional glass. Computational modeling is a promising tool to probe microstructural mechanics, but such studies in the literature are scarce. In this work, the theory of peridynamics, a non-local theory of continuum mechanics, is applied to simulate crack propagation through microstructural realizations of a model lithium-disilicate glass–ceramic. The crystalline and glassy phases within the microstructure are explicitly considered, with the size and shape of crystals inspired by experimental data. Multiple toughening mechanisms are revealed, which are functions of crystallinity and morphology, and the impact on fracture toughness is demonstrated. Crack path tortuosity is studied, and it is found that an optimum level of crack path tortuosity can be obtained in the range of 0.6–0.8 crystallinity. Numerical results are shown to agree well with previously published experimental and modeling results.     

Crack Tip Morphology of Slowly Growing Cracks in Glass

We present atomic force microscopy (AFM) observations of crack tips in glass during subcritical propagation. These have been obtained by means of an AFM sample holder which has been specially designed to propagate indentation cracks in glass plates. Crack tips in soda–lime–silica glass are always preceded by a few nanometers deep deformation. In vitreous silica, no other surface deformation than the crack itself could be detected. For both materials, the crack opening is found to largely exceed the elastic solution.     

Microstructure and ion-exchange properties of transparent glass-ceramics containing Zn2TiO4/α-Zn2SiO4 nanocrystals

Transparent glass-ceramics have particular properties compared with their precursor glasses, and have promising potential applications in many fields. Titanium-relative phases are frequently employed as nucleation agents for crystallization of glass-ceramics, and rarely been precipitated as functional nanocrystalline phases in glass-ceramics. In this work, transparent glass-ceramics containing Zn₂TiO₄ and/or α-Zn₂SiO₄ nanocrystals are investigated. It turns out that Vickers hardness of these glass-ceramics increases with the precipitation of Zn₂TiO₄ and α-Zn₂SiO₄ nanocrystals. Despite the blocking effect of nanocrystals precipitated in the glass-ceramics, structural and compositional modification of the residual glass induced by the precipitation of these nanocrystalline phases facilitates the K-Na ion-exchange, leading to the enhanced depth of layer and further improved Vickers hardness of the glass-ceramics.     

Toward hard and highly crack resistant magnesium aluminosilicate glasses and transparent glass-ceramics

High hardness and high crack resistance are usually mutually exclusive in glass materials. Through the aerodynamic levitation and laser melting technique, we prepared a series of magnesium aluminosilicate glasses with a constant MgO content, and found a striking enhancement of both hardness and crack resistance with increasing Al₂O₃. The crack resistance of the magnesium aluminosilicate glass is about five times higher than that of the binary alumina-silica glass for the similar [Al]/([Al] + [Si]) molar ratio (around 0.6). For the selected magnesium aluminosilicate glass with R = 0.32, when subjected to isothermal treatment at 1283K, we observed a further drastic enhancement of both hardness and crack resistance by extending the heating time. Based on the structural analyses, we propose an atomic-scale model to explain the mechanism of synergetic enhancement in hardness and crack resistance for the magnesium aluminosilicate glasses and glass-ceramics.     

Crack Growth in Soda–Lime–Silicate Glass near the Static Fatigue Limit

The atomic force microscope (AFM) was used to explore the nature of features formed on the surfaces of cracks in soda–lime–silicate glass that were held at stress intensity factors below the crack growth threshold. All studies were conducted in water. Cracks were first propagated at a stress intensity factor above the crack growth threshold and then arrested for 16 h at a stress intensity factor below the threshold. The stress intensity factor was then raised to reinitiate crack growth. The cycle was repeated multiple times, varying the hold stress intensity factor, the hold time, and the propagation stress intensity factor. Examination of the fracture surface by optical microscopy showed surface features that marked the points of crack arrest during the hold time. These features were identical to those reported earlier by Michalske in a similar study of crack arrest. A study with the AFM showed these features to be a consequence of a bifurcation of the crack surface. During the hold period, waviness developed along the crack front so that parts of the front propagated out of the original fracture plane, while other parts propagated into the plane. Crack growth changed from the original flat plane to a bifurcated surface with directions of as much as 3° to 5° to the original plane. This modification of crack growth behavior cannot be explained by a variation in the far-field stresses applied to the crack. Nor can the crack growth features be explained by chemical fluctuations within the glass. We speculate that changes in crack growth direction are a consequence of an enhancement in the corrosion rate on the flank of the crack at stresses below the apparent crack growth threshold in a manner described recently by Chuang and Fuller.     

Hertzian crack propagation in graded glass/ceramic composites

In literature, the concept of material gradation is shown to inhibit surface crack initiation in glass/ceramic composites subjected to Hertzian indentation. However, surface cracks could yet initiate due to relatively higher loadings or in the presence of surface flaws/defects. Hence, characterization of graded composites concerning the resistance against Hertzian crack initiation and propagation manifests itself as a prominent matter. In this study, axisymmetric Hertzian cracks evolving in graded glass/ceramic composites propelled by a rigid cylindrical punch are investigated employing a novel recursive method, called the stacked-node propagation procedure. Crack trajectories and their propagation susceptibilities are predicted via the minimum strain energy density (MSED) criterion regarding the crack growth resistance (R-curve) of ceramics. The stress trajectory approach is also considered for a homogeneous glass to reveal the reliance and effectiveness of the MSED criterion in the present crack problems. The Mori–Tanaka relations are adopted to model the elastic modulus and Poisson's ratio variations through the composites, which are implemented on the simulations via the homogeneous finite element approach. Hertzian crack problem of a practically producible graded composite comprised of oxynitride glass and a fine-grained silicon nitride ceramics (Si₃N₄) is treated as a case study. The degree of material gradation is assessed for the mitigation of surface crack initiation and propagation risks.     

Measurement of Very Slow Crack Growth in Glass

The rate of very slow crack growth in glass is measured by inducing small, controllable changes in the direction of propagation of Hertzian cone cracks at known times. After completion of a growth sequence, the sample is sectioned to reveal the fracture surface. The stress intensity factor at each stage of crack growth is calculated by using finite-element modeling of the stresses near the crack tip. Data are presented for crack growth velocities as low as 10⁻¹⁴ m/s in soda–lime glass. These data provide strong evidence for the existence of a subcritical limit for crack growth in this material.     

铁对R_2O-CaO-gO-Al_2O_3-SiO_2系玻璃微晶化的影响

就石材锯切粉在微晶玻璃中应用的主要问题—铁对析晶的影响展开研究。结果表明,少量铁(＜2mol%)的引入,可能引起析晶参数的升高,但外加铁含量超过2mol%时均可降低析晶参数,并使起始析晶至析晶峰的温度区间(Tp-Tg)变窄；外加铁量＜2mol%时,不同含铁量配方的(Tp-Tg)区间重叠显著,可以采用同一温度晶化处理；配方含铁与否对主晶相没有明显影响,但影响玻璃的析晶能力,铁含量＜2mol%时,使玻璃体析晶能力增加,接近或大于3mol%时,玻璃析晶能力降低；微粉制备微晶玻璃可以大幅度缩短晶化时间。     

铁对R2O-CaO-MgO-Al2O3-SiO2系玻璃微晶化的影响

就石材锯切粉在微晶玻璃中应用的主要问题-铁对析晶的影响展开研究。结果表明，少量铁（〈2mol％）的引入，可能引起析晶参数的升高，但外加铁含量超过2mol％时均可降低析晶参数，并使起始析晶至析晶峰的温度区间（Tp-Tg）变窄；外加铁量〈2mol％时，不同含铁量配方的（Tp—Tg）区间重叠显著，可以采用同一温度晶化处理；配方含铁与否对主晶相没有明显影响，但影响玻璃的析晶能力，铁含量〈2mol％时，使玻璃体析晶能力增加，接近或大于3mol％时，玻璃析晶能力降低；微粉制备微晶玻璃可以大幅度缩短晶化时间。     

Crack Propagation Through Interfaces in a Borosilicate Glass and a Glass Ceramic

Dynamic crack propagation across an adhesive interface in a borosilicate glass and a glass ceramic was studied to understand the interactions of cracks with the interface. Specimens were manufactured by attaching a notched plate to a rectangular plate using an epoxy adhesive. A plastic projectile was impacted on the notched edge to initiate a single crack at the notch tip in the first plate. The propagation of the crack in the first plate and the crack patterns after the interface in the second plate were recorded using a high-speed camera. For borosilicate glass, a single crack propagated to the adhesive interface and arrested for a certain time. Cracks re-initiated in the second plate, and crack patterns were observed to depend on the thickness of the adhesive interface. The crack developed a higher number of branches, and the branching angle increased as the interface thickness was increased. For the glass ceramic, the notch-initiated crack branched in the first plate and did not penetrate through to the second plate regardless of the various adhesive thicknesses studied.