Hardness, Toughness, and Scratchability of Germanium–Selenium Chalcogenide Glasses

Ge–Se chalcogenide glasses are characterized by relatively low hardness (0.39–2.35 GPa) and low fracture toughness (0.1–0.28 MPa·m^1/2). Actually, the hardness of chalcogen-rich glasses is low enough so that the brittleness parameter, B = H / K _c , is lower than that of silicate glasses. Whereas hardness and Young's modulus increase with increasing germanium contents, fracture toughness follows a trend similar to that of the density and exhibits a maximum for the Ge₂₀Se₈₀ composition, which corresponds to the rigidity percolation threshold. Optical microscopy and atomic force microscopy observations suggest that the indentation deformation proceeds by a localized shear deformation phenomenon. Glasses in the chalcogen-rich region behave viscoelastically at room temperature. As a consequence, an increase of the loading time results in a decrease of hardness and toughness.     

Effect of Indenter Geometry on Controlled-Surface-Flaw Fracture Toughness

Fracture toughness values obtained using both Knoop and Vickers-indentation-produced controlled surface flaws were compared as a function of indentation load for a well-characterized glass-ceramic material. At the same indentation load, Knoop cracks were larger than Vickers. As-indented K_c values calculated from fracture mechanics expressions for surface flaws were higher for Knoop flaws than Vickers, but both types gave low K_c values due to indentation residual stress effects. Analysis suggested that theoretical formalisms for indentation residual stress effects based on fracture mechanics solutions for a center-loaded penny crack in an infinite medium should apply to both indentation types. K_c values calculated using the residual stress approach were identical for Knoop and Vickers controlled surface flaws when a "calibration" value for a constant term in the expression for K_c was used for both indentation types.     

Cyclic Fatigue Life and Crack-Growth Behavior of Microstructurally Small Cracks in Magnesia-Partially-Stabilized Zirconia Ceramics

Cyclic fatigue stress/life ( S / N ) and crack-growth properties are investigated in magnesia-partially-stabilized zirconia (Mg-PSZ), with particular reference to the role of crack size. The material studied is subeutectoid aged to vary the steady-state fracture toughness, K_c , from ∼3 to 16 MPa · m^1/2· S / N data from unnotched specimens show markedly lower lives under tension—compression compared with tension—tension loading; "fatigue limits"(at 10⁸ cycles) for the former case approach 50% of the tensile strength. Under tension—tension loading, cyclic crack-growth rates of "long"(> 3 mm) cracks are found to be power-law dependent on the stress-intensity range, Δ K , with a fatigue threshold, Δ K _TH, of order 50% of K_c . Conversely, naturally occurring "small"(1 to 100 μm) surface cracks are observed to grow at Δ K levels 2 to 3 times smaller than Δ K _TH, similar to behavior widely reported for metallic materials. The observed small-crack behavior is rationalized in terms of the restricted role of crack-tip shielding (in PSZ from transformation toughening) with cracks of limited wake, analogous to the reduced role of crack closure with small fatigue cracks in metals. The implications of such data for structural design with ceramics are briefly discussed.     

Preparation, Hardness, and Fracture Toughness of Tantalum Oxynitride Ceramics

Tantalum oxynitride powder with a baddeleyite crystal structure was synthesized and densified by hot pressing in Ar and under high pressure using a belt-type high-pressure apparatus. The tantalum oxynitride powder could not be densified completely under hot-pressing conditions at 1400°C. The use of high pressure resulted in dense materials. The samples showed a hardness of 16–17 GPa and a fracture toughness of 3–4 MPa·m^1/2. The hardness is higher compared with that of ZrO₂ and HfO₂ ceramics. The fracture toughness corresponds to the value of fully stabilized ZrO₂ due to the absence of any transformation toughening mechanism.     

Toughening by Monoclinic Zirconia

The toughening induced by monoclinic ZrO₂ in the absence of microcracking was investigated, using ZnO as the host material. Toughness levels K_c in excess of the host toughness K_c^M were achieved, attaining a peak toughness K_c/K_c^M ∼1.7, at monoclinic ZrO₂ volume concentrations 0.2. This toughening is attributed to crack/particle interactions, associated with the deflection and bowing of the crack by the residual strain field around the monoclinic ZrO₂ particles.     

Microhardness and Fracture Toughness Anisotropy in Cubic Zirconium Oxide Single Crystals

Vickers and Knoop indentation tests have been used to study the fracture and deformation characteristics of 9.4-mol%-Y₂O₃-stabilized ZrO₂ single crystals. K_c is anisotropic, with values of 1.9 and 1.1 MPa·m^1/2 for radial cracks propagating along (100) and (110), respectively. The toughness for these two orientations was also determined using the single-edge notched-beam geometry, and yielded values of 1.9 and 1.5 MPa·m^1/2.     

Temperature–Time–Mechanical Properties of Glass–Ceramics Produced from Coal Fly Ash

Physical and mechanical properties of glass–ceramics fabricated from thermal power plant fly ash were analyzed and compared with suggest a temperature–time–mechanical (T–T–M) diagram. Coal fly ash with SiO₂–Al₂O₃–MgO–CaO as major components and TiO₂ as a nuclear agent were used to develop glass–ceramic materials which were heat treated at 900°–1050°C for 0.5–4 h for crystallization. It was verified that the high aspect ratio of unknown crystallines in the microstructure contributed high hardness, strength, fracture toughness, and wear resistance. These results are correlated with heat treatment conditions and microstructure and a T–T–M properties (hardness, strength, elastic constant, toughness, and wear rate) diagram on glass–ceramics produced from coal fly ash is proposed.     

Contact-induced Damage in Ceramic Coatings on Compliant Substrates: Fracture Mechanics and Design

Simple explicit relations are presented for the onset of competing fracture modes in ceramic coatings on compliant substrates from Hertzian-like contacts. Special attention is given to a deleterious mode of radial cracking that initiates at the lower coating surface beneath the contact, in addition to traditional cone cracking and quasiplasticity in the near-contact area. The critical load relations are expressed in terms of well-documented material parameters (elastic modulus, toughness, hardness, and strength) and geometrical parameters (coating thickness and sphere radius). Data from selected glass, Al₂O₃ and ZrO₂ coating materials on polycarbonate substrates are used to demonstrate the validity of the relations. The formulation provides a basis for designing ceramic coatings with optimum damage resistance.     

Micromechanical Model for Fibrous Ceramic Bodies

A micromechanical model is presented to relate the mechanical properties of low-density fibrous ceramic bodies to their micro-structures and the properties of the fibers. It is found that properties such as the elastic moduli, fracture toughness, and strength depend on the fiber spacing. In particular, it is shown that the critical stress intensity ( K_c ) depends on the density of the body with respect to the fiber density, the degree of preferred orientation, the fiber strength, and the fiber radius, suggesting ways of increasing K_c . Furthermore, it is predicted that K_c will be related to the sonic velocity in the material, reflecting variations in the degree of preferred orientation. The model is found to be consistent with the experimental observations on a silica-based fibrous ceramic, which is being used in the thermal protection system of the Space Shuttle.     

Mixed-Mode Fracture Toughness of Ceramic Materials

An experimental technique whereby pure mode I, mode II, and combined mode I-mode II fracture toughness values of ceramic materials can be determined using four-point bend specimens containing sharp, through-thickness precracks is discussed. In this method, notched and fatigue-precracked specimens of brittle solids are subjected to combined mode I-mode II and pure mode II fracture under asymmetric four-point bend loading and to pure mode I under symmetric bend loading. A detailed finite element analysis of the test specimen is performed to obtain stress intensity factor calibrations for a wide range of loading states. The effectiveness of this method to provide reproducible combined mode I-mode II fracture toughness values is demonstrated with experimental results obtained for a polycrystalline Al₂O₃. Multiaxial fracture mechanics of the Al₂O₃ ceramic in combined modes I, II, and III are also described in conjunction with the recent experimental study of Suresh and Tschegg (1987). While the mode II fracture toughness of the alumina ceramic is comparable to the mode I fracture toughness K _Ic, the mode III fracture initiation toughness is 2.3 times higher than K _Ic. The predictions of fracture toughness and crack path based on various mixed-mode fracture theories are critically examined in the context of experimental observations, and possible effects of fracture abrasion on the apparent mixed-mode fracture resistance are highlighted. The significance and implications of the experimental methods used in this study are evaluated in the light of available techniques for multiaxial fracture testing of brittle solids.     

Processing Temperature Effects on Molybdenum Disilicide

A series of MoSi₂ compacts were fabricated at increasing hot-pressing temperatures to achieve different grain sizes. The materials were evaluated by Vickers indentation fracture to determine room-temperature fracture toughness, hardness, and fracture mode. From 1500° to 1800°C, MoSi₂ had a constant 67% transgranular fracture and linearly increasing grain size from 14 to 21 μm. Above 1800°C, the fracture percentage increased rapidly to 97% transgranular at 1920°C (32-μm grain size). Fracture toughness and hardness decreased slightly with increasing temperature. MoSi₂ processed at 1600°C had the highest fracture toughness and hardness values of 3.6 MPa.m^1/2 and 9.9 GPa, respectively. The effects of SiO₂ formation from oxygen impurities in the MoSi₂ starting powders and MoSi₂–Mo₅Si₃ eutectic liquid formation were studied.     

Anisotropy of Fracture Toughness of Piezoelectric Ceramics

The anisotropy of fracture toughness of PZT- and barium titanate-based piezoelectric ceramics was studied using doubletorsion and indentation methods. The influence of elastic anisotropy and the piezoelectric effect in calculating the K_c value are discussed. The fracture toughness in the polarization plane is greater than that in the perpendicular plane. A model is suggested to explain the observed anisotropy; it is based on assumption of a stress-induced domain reorientation zone near the crack tip.     

Cyclic Fatigue-Crack Growth and Fracture Properties in Ti3SiC2 Ceramics at Elevated Temperatures

The cyclic fatigue and fracture toughness behavior of reactive hot-pressed Ti₃SiC₂ ceramics was examined at temperatures from ambient to 1200°C with the objective of characterizing the high-temperature mechanisms controlling crack growth. Comparisons were made of two monolithic Ti₃SiC₂ materials with fine- (3–10 μm) and coarse-grained (70–300 μm) microstructures. Results indicate that fracture toughness values, derived from rising resistance-curve behavior, were significantly higher in the coarser-grained microstructure at both low and high temperatures; comparative behavior was seen under cyclic fatigue loading. In each microstructure, Δ K _th fatigue thresholds were found to be essentially unchanged between 25° and 1100°C; however, there was a sharp decrease in Δ K _th at 1200°C (above the plastic-to-brittle transition temperature), where significant high-temperature deformation and damage are first apparent. The substantially higher cyclic-crack growth resistance of the coarse-grained Ti₃SiC₂ microstructure was associated with extensive crack bridging behind the crack tip and a consequent tortuous crack path. The crack-tip shielding was found to result from both the bridging of entire grains and from deformation kinking and bridging of microlamellae within grains, the latter forming by delamination along the basal planes.     

Impact Damage and Strength Degradation in a Silicon Carbide Reinforced Silicon Nitride Composite

Adding SiC particles to Si₃N₄ and subjecting the mixture to a sinter-hot-isostatic-pressing process increases both the strength and elastic modulus. It also decreases the hardness but maintains the fracture toughness, which results in a higher resistance to crack initiation and propagation during spherical particle impact. Sinter-hot-isostatically-pressed composites exhibit elastic response as their dominant behavior. They also display a high resistance to Hertzian cone crack initiation and extension. This is due to the increased degree of inelastic deformation of sinter-hot-isostatically-pressed composites.     

High-Toughness Silicon Carbide as Armor

Silicon carbide, with single-edge precracked beam (SEPB) toughness greater than 7 MPa·m^1/2, was made by hot-pressing using Al–B–C (ABC) or Al–Y₂O₃ (YAG) as additives. The hardness of SiC processed with a liquid phase was always less than SiC densified without a liquid phase despite having a similar or finer grain size. With increasing Al content, the ABC system changed from trans- to intergranular fracture with a drop in hardness and a two- to threefold increase in SEPB toughness. Strength and Weibull modulus for materials processed with a liquid phase were higher than those of solid-state densified SiC. Ballistic testing, however, did not show any improvement over SiC densified with B and C additives. Depth of penetration was controlled by hardness of the SiC-based materials, while V ₅₀ values for 14.5 mm WC–Co cored projectiles were in the range of 720–750 m/s for all materials tested.     

On the Vickers Indentation Fracture Toughness Test

The Vickers indentation fracture toughness test, or VIF, is addressed by considering its origins and the numerous equations that have been applied along with the technique to estimate the fracture resistance, or the K _{I c} of ceramics. Initiation and propagation of cracks during the VIF test are described and contrasted with the pre-cracking and crack growth for internationally standardized fracture toughness tests. It is concluded that the VIF test technique is fundamentally different than standard fracture toughness tests. The VIF test has a complex three-dimensional crack system with substantial deformation residual stresses and damage around the cracks. The VIF test relates to an ill-defined crack arrest condition as opposed to the rapid crack propagation of the standardized fracture toughness tests.
Previously published fracture toughness results employing the VIF technique are reviewed. These reveal serious discrepancies in reported VIF fracture toughness values. Finally, recent fracture resistance measurements by the VIF technique for the Standard Reference Material SRM 2100 are presented. These are compared with standardized test results for the same material. It is concluded that the VIF technique is not reliable as a fracture toughness test for ceramics or for other brittle materials. What the VIF actually measures in terms of fracture resistance cannot be readily defined. It is recommended that the VIF technique no longer be acceptable for the fracture toughness testing of ceramic materials.     

Measurement of Dynamic Hardness by Controlled Sharp-Projectile Impact

Impact of ZnS by a pyramidal projectile was used to provide a measurement of the dynamic hardness and to obtain direct comparison of the contact damage produced by static loading and impact. The dynamic hardness was evaluated from measurements of residual contact dimensions as a function of impact velocity, over the velocity range 5 to 40 m.s^-1. The value obtained ( H_d =5.0 GPa) was higher than the static hardness ( H_S = 1.9 GPa). The higher hardness in impact causes more extensive cracking, an increase in the elastic recovery of the depth of the residual contact impression, and a smaller plastic zone surrounding the contact site. The relative extents of cracking in impact and static loading are predicted by a quasistatic indentation fracture mechanics analysis along with the appropriate values of hardness.     

Effect of Subcritical Crack Growth on Fracture Toughness and Work-of-Fracture Tests Using Chevron-Notched Specimens

A correlation between the plane strain stress intensity factor K_I , load, and crack extension has been analyzed for constant displacement and constant loading rate experiments, using chevron-notched, four-point-bend specimens. It is assumed that at the beginning of the experiment the chevron triangle tip is not ideally sharp. As loading continues, the crack initially moves with velocity v_t at K_I equal to a threshold value K_t . Maximum crack velocity is reached at K_I= K_IC , the fracture toughness. Depending on the type of material tested, a specific displacement or loading rate must be used to correlate the maximum load with K_Ic . An error in K_IC calculation is estimated if different displacement rates are applied. Repeated loading-unloading work-of-fracture (WOF) experiments generate values related to the resistance of the material to fracture initiation, K_t , only when the crack length approaches 100% of the specimen width. Values related to material's fracture toughness, K_IC are not generated in WOF tests.     

Influence of Test Methods on Fracture Toughness of a Dental Porcelain and a Soda Lime Glass

The aim of this study was to investigate the influence of the test method on fracture toughness of a dental porcelain and a soda lime glass. Three methods were used to determine fracture toughness: the indentation strength (IS) by bending, chevron-notched beam (CNB), and the single-edge-notched beam (SENB). In the IS method, the ratio of elastic modulus to hardness ( E / H ) in the formula was determined by two methods: individual measurement for E and H (IS_M) as well as direct estimation from Knoop's indentation method (IS_K). The tested materials were a dentin porcelain, a traditional feldspar-based leucite-reinforced glass ceramic (Carrara Vincent), and a soda lime glass. Carrara Vincent showed a higher toughness ( P <0.01) than glass with all three test methods. The toughness values manifested significant differences between the methods used ( P <0.01). The two-way analysis of variance suggested that the materials tested and the test methods used had interaction effects, which statistically means that differences in materials and methods influenced the comparability of the toughness result. In this study, a first step was made to compare different toughness test methods by testing the toughness of a traditional feldspar-based leucite-reinforced glass ceramic and a soda lime glass that has a homogeneous microstructure. An interaction effect of the method and the material used was shown. As a consequence, none of the methods tested is suitable as a universal fracture toughness test method. Further research is needed to investigate more extensively the influence of material composition on the fracture toughness test methods' comparability.