Fracture Toughness of Dental Porcelains Evaluated by IF, SCF, and SEPB Methods

Fracture toughness of six dental porcelains with leucite content ranging from 0 to 22 vol% was evaluated by indentation fracture (IF), surface crack in flexure (SCF), and single edge pre-cracked beam (SEPB) methods. The results of the IF method were similar to those of the SCF method for all the porcelains investigated. The results of the SEPB were similar to those of the other two methods only for the glassy porcelains, but for leucite-based porcelains this method resulted in higher values of K _{I c} . Based on microstructure, fractographic analysis, and an additional single edge V-notched beam test, it was concluded that the pre-crack size influences the value of K _{I c} for porcelains reinforced by leucite. For design and failure analysis purposes, the K _{I c} determined by SCF method should be preferred, since fracture of dental restorations usually starts from small surface cracks.     

Measurement of Fracture Toughness of Plasma-Sprayed Al2O3 Coatings Using a Tapered Double Cantilever Beam Method

The fracture toughness of plasma-sprayed Al₂O₃ coatings in terms of the critical strain energy release rate G _Ic was measured using a tapered double cantilever beam (TDCB) approach. The fracture surfaces were examined using a scanning electron microscope (SEM). The measurement yielded the mean G _Ic values from 13 to 27 J/m² for the sprayed Al₂O₃ coatings at different spray distances. These values agree well with those obtained by the conventional double cantilever beam approach. The dependence of the observed G _Ic on spray distance is consistent with that for the lamellar bonding ratio. These results suggest that the TDCB test is a reliable approach for measuring the G _Ic of thermal-spray coatings without the crack-length measurement.     

VAMAS Round Robin on Fracture Toughness of Silicon Nitride

Eight laboratories in Germany, Japan, U.K., and U.S. participated in the VAMAS round robin. The fracture toughness of silicon nitride at room temperature and at 1200^deg;C was measured by three methods: the single-edge V-notched beam (SEVNB), single-edge precracked beam (SEPB), and chevron notched beam (CNB). The obtained values show hardly any crosshead speed dependence, irrespective of test temperature and atmosphere. Results may have been influenced by a small amount of slow crack growth, but distinct R -curve behavior could not be detected within the scope of the tests. The values at 1200^deg;C in N₂ can be measured by the SEVNB and SEPB methods with small scatters. The oxidation of silicon nitride, caused by heating in air, increases the SEVNB and SEPB values. The CNB values are free from the effects of test temperature and atmosphere, but they show a large scatter between laboratories. However, the chevron V-notched beam (CVNB) method, which is an improved CNB method, shows values with a small scatter, irrespective of the measurement conditions. The SEVNB and SEPB measurements in N₂ and the CVNB measurement under any conditions are recommended for the measurement of high-temperature fracture toughness.     

Comparison of KIc Values for Al2O3-ZrO2 Composites Obtained from Notched-Beam and Indentation Strength Techniques

Values of K_Icfor hot-pressed AL₂O₃-ZrO₂ composites were measured using notched-beam and indentation strength techniques. The results are compared with K factors at the mirror/mist boundary and at crack branching. It was found that the indentation strength technique provides a more consistent estimation of K_Ic, than the notched-beam technique.     

Effect of Crystallinity on Strength and Fracture Toughness of Li2O-Al2O3-CaO-SiO2 Glass-Ceramics

The influence of crystal volume fraction on fracture toughness ( K _{I C} ) and indentation strength was analyzed for Li₂O-Al₂O₃-CaO-SiO₂ (LACS) and LACS glass-ceramics containing 0.58 mmol% AgNO₃ (LACS-0.58Ag) or 0.78 mmol% AgNO₃ (LACS-0.78Ag). The mean flexure strength, indentation strength, and K_{I C} values of the LACS-0.78Ag groups increased with volume fraction of crystallinity. To achieve the greatest strength and K_{I C} in LACS-Ag specimens, a high volume fraction of crystallinity (95%) had to be produced. However, the relationship between volume fraction of crystal phase and translucency had to be analyzed to determine the influence of crystallization on the potential esthetic results that are essential for dental applications. Addition of AgNO₃ to LACS glass produced a change from surface crystallization to bulk crystallization.     

Indentation Damage and Residual Stress Field in Alumina-Y2O3-Stabilized Zirconia Composites

Fracture features, residual stresses, and zirconia transformation are studied in indentation strength specimens of alumina-Y₂O₃-stabilized zirconia (3% mol of Y₂O₃, 3YTZP) ceramics in order to analyze the extension of the indentation damage in the bulk of the specimens. Two compositions, 5 vol% 3YTZP (A5) and 40 vol% 3YTZP (A40), have been prepared by stacking tape-casted tapes and sintering. After indentation with loads ranging from 50 to 300 N, samples were fractured in four-point bending and the fracture surfaces were characterized by scanning electron microscopy. Raman and piezospectroscopic techniques were used to determine the monoclinic zirconia fraction and the residual stresses through the fracture surfaces. In the A5 composition, the indentation damage morphology was clearly half-penny, whereas the A40 composition presented Palmqvist crack formation. Zirconia transformation was only observed in the plastically deformed zones underneath the imprints whereas there were significant residual compressive stresses outside the plastic zones due to the indentation damage. The intensity of this residual compressive field was dependent on the level of zirconia transformation due to indentation damage because zirconia transformation induced tensile stress fields superimposed on the compressive stresses.     

Fracture Toughness Determination of A12O3 Using Four-Point-Bend Specimens with Straight-Through and Chevron Notches

Fracture toughness of a sintered A1₂O₃ was determined with four-point-bend specimens having either straight-through or chevron notches. For the straight-through notched specimens, measured K _Ic decreased with decreasing notch width. For the smallest notch width (66 μm) K _Ic= 3.42±0.13 MN m^−¾. For specimens with chevron notches, a crack initiates and extends from the tip of the notch under increasing load. K _Ic is calculated from the maximum load without measuring crack length, under the assumption that the derivative of the compliance is the same as that for a specimen with a straight-through crack. A refined calculation accounts for the truncated chevron crack shape at maximum load using Bluhm's slice model. For the chevronnotch configuration, a value of K _Ic= 3.49±0.11 MN m^−¾ was measured, which appears to be independent of the initial notch length a ₀ (distance from the crack mouth to the tip of the triangular notch). An effect of a ₁ (length of the chevron notch at the surface) on K _Ic was observed, independent of whether the calculation of K _Ic was based on the straight-through crack assumption or on the slice model.     

Indentation Fracture Response and Damage Resistance of Al2O3-ZrO2 Composites Strengthened by Transformation-Induced Residual Stresses

Indentation fracture behavior of three-layer Al₂O₃-ZrO₂ composites with substantial compressive residual stresses was compared with the behaviors of monolithic Al₂O₃ and Al₂O₃-ZrO₂ ceramics without intentionally introduced residual stresses. The indentation cracks were smaller in the three-layer specimens relative to the monolithic specimens in agreement with the predictions of indentation fracture mechanics theory. Indentation and strength testing were used to show that a residual compressive stress of approximately 500 MPa exists in the outer layers of the three-layer composites. The three-layer specimens showed excellent damage resistance in that the strength differential between the three-layer and monolithic indented specimens was maintained at indentation loads up to 1000 N, the maximum indentation load used in the experiments.     

Effects of Residual Stress and Loading Geometry on Single-Edge Precracked-Beam (SEPB) Fracture-Toughness Test Results

The single-edge precracked-beam (SEPB) specimen test, using the "bridge indentation" method, is one of the standard test methods in the new ASTM standard for the determination of the fracture toughness of ceramics. In support of this effort, the effect of several test parameters on the fracture-toughness ( K _{I C} ) values was established. The effect of the residual stress, because of the indent and the alignment in three- and four-point bending, on the K _{I C} values was determined using aluminum nitride specimens. The results show that indent loads should be kept below 10 kgf, and the crack-plane angle should be <5°, to prevent artificially high K _{I C} values.     

Controlled Surface Flaws in Hot-Pressed Si3N4

Surface flaws of controlled size and shape were produced in high-strength hot-pressed Si₃N₄ with a Knoop microhardness indenter. Fracture was initiated at a single suitably oriented flaw on the tensile surface of a 4-point-bend specimen, with attendant reduction in the measured magnitude and scatter of the fracture strength. The stress required to propagate the controlled flaw was used to calculate the critical stress-intensity factor, K _IC, from standard fracture-mechanics formulas for semielliptical surface flaws in bending. After the bend specimen had been annealed, the room-temperature K _IC values for HS-130 Si₃N₄ increased to a level consistent with values obtained from conventional fracture-mechanics tests. It was postulated that annealing reduces the residual stresses produced by the microhardness indentation. The presence of residual stresses may account for the low K _IC, values. Elevated-temperature K_IC values for HS-130 Si₃N₄ were consistent with double-torsion data. Controlled flaws in HS-130 Si₃N₄ exhibited slow crack growth at high temperatures.     

Formation, Characterization, and Hot Isostatic Pressing of Cr2O3-Doped ZrO2 (0,3 mol% Y2O3) Prepared by Hydrazine Method

In the ZrO₂-Cr₂O₃ system, metastable t -ZrO₂ solid solutions containing up to 11 mol% Cr₂O₃ crystallize at low temperatures from amorphous materials prepared by the hydrazine method. The lattice parameter c decreases linearly from 0.5149 to 0.5077 nm with increased Cr₂O₃ content, whereas the lattice parameter a is a constant value ( a = 0.5077 nm) regardless of the starting composition. At higher temperatures, transformation (decomposition) of the solid solutions proceeds in the following way: t (ss)→ t (ss) + m + Cr₂O₃→ m + Cr₂O₃. Above 11 mol% Cr₂O₃ addition, c-ZrO₂ phases are formed in the presence of Cr₂O₃. The t -ZrO₂ solid solution powders have been characterized for particle size, shape, and surface area. They consist of very fine particles (15–30 nm) showing thin platelike morphology. Dense ZrO₂(3Y)-Cr₂O₃ composite ceramics (∼99.7% of theoretical) with an average grain size of 0.3 μm have been fabricated by hot isostatic pressing for 2 h at 1400°C and 196 MPa. Their fracture toughness increases with increased Cr₂O₃ content. The highest K _Ic value of 9.5 MPa·;m^1/2 is achieved in the composite ceramics containing 10 mol% Cr₂O₃.     

Indentation of Silicate-Glass Films on Al2O3 Substrates

The deformation of thin layers of glass on crystalline materials has been examined using newly developed experimental methods for nanomechanical testing. Continuous films of anorthite (CaAl₂Si₂O₈) were deposited onto Al₂O₃ surfaces by pulsed-laser deposition. Mechanical properties such as Young's modulus and hardness were probed with a high-resolution depth-sensing indentation instrument. Nanomechanical testing, combined with AFM in situ imaging of the deformed regions, allowed force-displacement measurements and imaging of the same regions of the specimen before and immediately after indentation. This new technique eliminates any uncertainty in locating the indentation after unloading. Emphasis has been placed on examining how the Al₂O₃ substrate crystallographic orientation will affect mechanical composite response of silicate-glass film/Al₂O₃ system.     

Short-Crack Fracture Toughness of Silicon Carbide

The fracture toughness of four different silicon carbides was measured using single-edge precracked beam (SEPB) and indentation/strength techniques. Two were development grades with similar microstructures and chemistries, and yet exhibited different fracture modes. The grade that exhibited a predominantly intergranular fracture had an SEPB fracture toughness (6.4 MPa√m) 88% higher than the one that showed primarily a transgranular fracture (3.4 MPa√m). The higher fracture toughness was associated with a modest increase in average strength (25%), although there was a significant increase in the Weibull modulus (11–32). Fracture toughness at short crack lengths was assessed by an indentation method that used fracture strengths, crack lengths at fracture, and a new method of estimating the constant δ that characterizes the residual driving force of the plastic zones based on the stable growth of the indentation cracks from the initial ( c ₀) to the instability ( c ^*) lengths. The results showed a rising crack-growth-resistance behavior for the grade exhibiting intergranular fracture, while the grade showing transgranular fracture had a flat crack-growth resistance. Tests on two commercial grades of silicon carbide showed similar behaviors associated with the respective fracture modes.     

Fracture toughness of (Ce) stabilized ZrO2/Al2O3 composites

Three techniques for the determination of K_Ic in Ce-stabilized ZrO₂/Al₂O₃ composites have been evaluated: the single-edge-notched beam (SENB); the indentation strength in bending (ISB) and the indentation fracture (IF). Comparative measurements, performed on samples prepared by sintering uniaxially pressed powders obtained by a chemical route, showed that whatever the technique used, K_Ic increased as the Al₂O₃ grain size decreased.

The three methods give similar results if some procedural improvements are introduced, namely: (i) the polished samples are annealed prior to testing: (ii) a more reproducible notching technique would be developed for the SENB method; and (iii) the crack shape and length are known exactly in the IF technique.

In the IF test, the crack shape profile is of Palmquist type at low indentation loads while a transition to a half-penny-shaped crack occurs at higher loads.     

Indentation Studies on Y2O3-Stabilized ZrO2: II, Toughness Determination from Stable Growth of Indentation-Induced Cracks

Stable indentation cracks were grown in four-point bend tests to study the fracture toughness of two Y₂O₃-stabilized ZrO₂ ceramics containing 3 and 4 mol% Y₂O₃. By combining microscopic in situ stable crack growth observations at discrete stresses with crack profile measurements, the dependence of toughness on crack extension was determined from crack extension plots, which graphically separate the crack driving residual stress intensity and applied stress intensity factors. Both materials exhibit steeply rising R -curves, with a plateau toughness of 4.5 and 3.1 Mpa·m^1/2 for the 3- and 4-mol% materials, respectively. The magnitude of the plateau toughness reflects the fraction of tetragonal grains contributing to transformation toughening.     

Fracture Modes in MoSi2

The room-temperature fracture behavior of polycrystalline MoSi₂ was characterized using Vickers indentation fracture. Fracture analysis was aided by the optically active grain structure of MoSi₂ revealed under polarized light. Radial crack propagation from indentations was found to be predominantly transgranular. The approximate indentation fracture toughness of MoSi₂ was 3 MPa.m^1/2, while the measured hardness was 8.7 GPa. Fracture behavior is believed to be controlled by anisotropy and cleavage energy of the tetragonal MoSi₂ crystal structure.     

Factor Analysis of Fracture-Toughness Test Parameters for Al2O3

The double-cantilever-beam technique was used to determine the effects of varying 6 factors related to specimen preparation, size, and testing conditions on the fracture toughness of polycrystalline Al₂O₃. Experimental design and statistical factor analysis techniques were used to investigate each factor at two levels. Direct fracture surface replication and electron microscopy provided supporting information about the fracture mode and fracture surface features for each test condition. The fracture toughness of Al₂O₃ was higher for 30-μm grain size than for 10-μm grain size. Pretest annealing (900°C) and specimen width were both significant factors for 10-μm Al₂O₃. The effects of variations of beam width, beam height, and test machine speed were masked by data scatter and are being studied further. The ratio of specimen width to fracture web width caused no effect in the range studied. The sensitivity of the test results to sample dimensions and surface finish is small enough that special care in cutting and measuring of samples is not required.     

Fracture Behavior of Directionally Solidified Y3Al5O12/Al2O3 Eutectic Fiber

The strength and fracture of a directionally solidified Y₃Al₅O₁₂/Al₂O₃ eutectic fiber were investigated. The fiber was grown continuously by an edge-defined film-fed growth technique. The microstructure was characterized using X-ray diffraction, scanning electron microscopy, and energy-dispersive spectroscopy. The tensile strength and Weibull's modulus of the eutectic fibers were determined in the as-fabricated state and after extended thermal exposure at 1460°C in air. Fractographic analysis was used to identify and classify the strength-limiting mechanisms. The fracture toughness and crack growth behavior were characterized by an indentation technique. A fracture mechanics analysis was also used to establish the relationships between surface flaw size, tensile strength, and fracture toughness of the fiber.     

Mixed-Mode Fracture of Hot-Pressed Si3N4

The mixed-mode fracture of hot-pressed Si₃N₄ was investigated using inclined indentation surface flaws in bending and large crack geometries in combined tension/torsion. Non-coplanar fracture was observed in all cases. Values of K_Ic, K_IIc, and K_IIIc stress intensity factors were obtained, with ratios K_IIc/K_Ic= 0.79 and K_IIIc/K_Ic= 1.55 observed. For large cracks, mode II conditions had more of an effect on mode I fracture than mode III conditions. The mixed-mode I-II fracture of surface flaws was significantly different from that for large cracks, suggesting surface flaw shear resistance effects. A model describing these effects was derived, based on the ratio of the crack-opening displacement to the crack surface asperity height.     

High-Temperature Mechanical Properties of SiC–Mo5(Si,Al)3C Composites

SiC–Mo₅(Si,Al)₃C composites were fabricated by the melt infiltration process, and the infiltration characteristics were studied in detail. Fracture strength and toughness were measured up to 1600°C using a three-point bending test and indentation strength method, respectively. Both fracture strength and toughness significantly increased at 1400°C with respect to the values at room temperature. These increases were mainly attributed to plastic deformation of the infiltrated Mo₅(Si,Al)₃C phases at elevated temperatures, which acted as ductile toughening inclusions. Compressive creep tests were used to study the creep behavior of the composite in the range of 1550°–1650°C and 150–200 MPa. The stress exponent and activation energy were 1.3 and 277 kJ/mol, respectively. Preliminary oxidation tests showed that the composites exhibited good oxidation resistance at 1500°C because of the formation of a dense oxide scale.