George D. Quinn

Indentation brittleness of ceramics: a fresh approach

The hardness and brittleness of ceramic materials are interrelated. Hard materials are more apt to fracture in the vicinity of an indentation during a hardness test, while softer materials tend to plastically deform to the indenter shape without fracturing. Measured hardness, in turn, is affected by both specimen deformation and fracture processes. This interrelationship is examined by means of extensive Vickers hardness testing. A new index of brittleness is proposed.

Fracture toughness (KIc) of a dental porcelain determined by fractographic analysis

OBJECTIVES Fractographic analysis of indentation cracks is performed following flexure testing as part of the ASTM (1999) standard for fracture toughness, KIc, determination in advanced ceramics. This method depends on the conduciveness of the material towards fractographic interpretation. The purpose of this study was to evaluate the use of fractography in fracture toughness methods with a feldspathic dental porcelain, in which KIc was measured fractographically as well as numerically using two controlled-flaw beam bending techniques. METHODS The following methods for KIc determination were applied to a dental porcelain containing a leucite volume fraction of 15-20%: (1) surface crack in flexure (SCF) (dependent upon fractographic analysis); and (2) indentation strength (IS) at indentation loads of 9.8 and 19.6 N (applying both standard numeric calculations and fractographic analysis). The testing environments were (1) ambient air (IS and SCF) and (2) flowing dry nitrogen (SCF). RESULTS No significant differences were found between numeric and fractographic KIc values for the IS technique at both indentation loads (9.8 and 19.6 N) in ambient air, although KIc values were sensitive to indentation load. Due to the presence of residual stresses, stable crack extension was observed fractographically in all IS specimens, as evidenced by differences between initial (ainitial) and critical (acritical) crack dimensions. For the SCF method, there was a significant difference in toughness between specimens tested in air versus dry nitrogen, however no fractographic evidence for chemically assisted slow crack growth (SCG) was observed. SIGNIFICANCE The SCF method as described by the ASTM standard was applicable to the feldspathic porcelain and produced very comparable results with the numeric toughness calculations of the IS procedure. However, fractographic analysis of the surface crack was somewhat difficult for this glassy ceramic compared with polycrystalline ceramics. Knowledge about stable crack extension or slow crack growth and its fractographic appearance is essential when estimating the toughness from examination of flaw dimensions on fractured surfaces since large calculation errors may occur if these effects are not taken into account.

Effect of Loading Rate Upon Conventional Ceramic Microindentation Hardness

The world standards for conventional ceramic hardness have varying requirements for control of loading rate during the indentation cycle. A literature review suggests that loading rate may affect measured hardness in some instances. In view of the uncertainty over this issue, new experiments over a range of indentation loading rates were performed on a steel, sintered silicon carbide, and an aluminum oxynitride. There was negligible effect upon Vickers hardness when loading rate was varied by almost four orders of magnitude from approximately 0.03 N/s to 10 N/s.

Fractographic failure analysis of a Procera AllCeram crown using stereo and scanning electron microscopy

OBJECTIVES Presentation of a methodological approach using stereo and scanning electron microscope examination for the failure analysis of an alumina all-ceramic premolar crown (Procera AllCeram). METHODS The recovered part of a fractured Procera alumina crown was examined utilizing first a stereomicroscope and second a scanning electron microscope (SEM). The stereomicroscope analysis was performed at low magnifications with oblique lighting in order to enhance spatial relationships and gross detection of crack features. A preliminary fracture surface map of the stereo observations was drawn and used as a guide for the SEM analysis that followed. Specific sites of interest identified under the stereo microscope were analyzed using the SEM at high magnifications searching for small fracture features such as wake hackle and twist hackle within the veneering ceramic in order to confirm the direction of crack propagation. RESULTS At low magnifications and oblique illumination, the stereomicroscope analysis provided an excellent overview of the fractured topography, showing sites of major interest such as a primary edge chip at a margin, a compression curl indicating the end of the fracture event as well as larger hackle lines distributed over the cracked surface. The greater magnifications with the SEM analysis of the sites of interest showed the presence of wake and twist hackle, indicators of the crack propagation direction. A general map of the fracture events could be reconstructed starting with a primary veneer edge chip at the mesial margin. Hackle and wake hackle of the crack front emanating from this margin arose from hoop stresses and propagated through the full crown thickness towards the distal end of the restoration where the compression curl was located. Additional occlusal surface damage in the form of veneer chipping containing arrest lines and twist hackle running in the opposite direction as the main crack path were observed, but occurred as a secondary event without penetrating the alumina core material. SIGNIFICANCE Stereo and scanning electron microscopy are complementary analysis techniques useful for the mapping and interpretation of the fracture surface. This case examination is intended to guide the clinical researcher in using qualitative (descriptive) fractography as a tool for understanding the failure process in brittle restorative materials, as well as for assessing possible design inadequacies.

Fracture toughness of advanced ceramics at room temperature

This report presents the results obtained by the five U.S. participating laboratories in the Versailles Advanced Materials and Standards (VAMAS) round-robin for fracture toughness of advanced ceramics. Three test methods were used: indentation fracture, indentation strength, and single-edge pre-cracked beam. Two materials were tested: a gas-pressure sintered silicon nitride and a zirconia toughened alumina. Consistent results were obtained with the latter two test methods. Interpretation of fracture toughness in the zirconia alumina composite was complicated by R-curve and environmentally-assisted crack growth phenomena.

Material properties and fractography of an indirect dental resin composite

OBJECTIVES Determination of material and fractographic properties of a dental indirect resin composite material. METHODS A resin composite (Paradigm, 3M-ESPE, MN) was characterized by strength, static elastic modulus, Knoop hardness, fracture toughness and edge toughness. Fractographic analyses of the broken bar surfaces was accomplished with a combination of optical and SEM techniques, and included determination of the type and size of the failure origins, and fracture mirror and branching constants. RESULTS The flexure test mean strength+/-standard deviation was 145+/-17 MPa, and edge toughness, T(e), was 172+/-12N/mm. Knoop hardness was load dependent, with a plateau at 0.99+/-0.02 GPa. Mirrors in the bar specimens were measured with difficulty, resulting in a mirror constant of approximately 2.6 MPa m(1/2). Fracture in the bar specimens initiated at equiaxed material flaws that had different filler concentrations that sometimes were accompanied by partial microcracks. Using the measured flaw sizes, which ranged from 35 to 100 microm in size, and using estimates of the stress intensity shape factors, fracture toughness was estimated to be 1.1+/-0.2 MPa m(1/2). SIGNIFICANCE Coupling the flexure tests with fractographic examination enabled identification of the intrinsic strength limiting flaws. The same techniques could be useful in determining if clinical restorations of similar materials fail from the same causes. The existence of a strong load-dependence of the Knoop hardness of the resin composite is not generally mentioned in the literature, and is important for material comparisons and wear evaluation studies. Finally, the edge toughness test was found promising as a quantitative measure of resistance to edge chipping, an important failure mode in this class of materials.

Fracture Mechanism Maps for Advanced Structural Ceramics. Part 1. Methodology and Hot-Pressed Silicon Nitride Results

The static fatigue behaviour of advanced structural ceramics can be controlled by a variety of failure mechanisms. A fracture mechanism map can define the stress-temperature regimes where the different mechanisms are dominant. The static fatigue resistance of a hot-pressed silicon nitride with magnesia sintering aid is limited by slow crack growth or creep fracture depending upon the specific stress-temperature conditions. The flexural fracture map is considerably refined relative to earlier versions, and in conjunction with available tension data, was used to create a tension fracture map. The fracture map brings together the findings of a number of studies and can be appreciated by materials scientists and engineers.

Comparison of edge chipping resistance of PFM and veneered zirconia specimens.

OBJECTIVES To investigate the chipping resistance of veneered zirconia specimens and compare it to the chipping resistance of porcelain fused to metal (PFM) specimens. METHODS Veneered zirconia and PFM bar specimens were prepared in clinically relevant thicknesses. The specimen edges were chipped with different magnitude forces, producing chips of various sizes. The range of sizes included small chips that did not penetrate all the way through the veneers to the substrates, and also chips that were very large and reached the zirconia or metal substrates. The relationship between force magnitude and chip size (edge distance) was graphed. The resulting curves were compared for the veneered zirconia and PFM specimens. Knoop hardness vs. force graphs for the veneers and substrates were also obtained. RESULTS The zirconia and PFM veneer chipping data followed a power law (coefficient of determination, R(2)>0.93) as expected from the literature. The curves overlapped within the combined data scatter, indicating similar resistance to chipping. The chips made in both types of specimens detached and did not penetrate into the substrate when they reached the veneer/substrate intersections. The hardness-load curves for the veneers and substrates all exhibited an indentation size effect (ISE) at low loads. The Knoop hardness values with uncertainties of +/-one standard deviation at 4N loads for the metal, zirconia, and the metal and zirconia veneers are: (2.02+/-0.08, 12.01+/-0.39, 4.24+/-0.16 and 4.36+/-0.02GPa), respectively, with no statistically significant difference between the veneers (Tukey pairwise comparison at 0.95 family confidence). SIGNIFICANCE This work indicates that a similar resistance to chipping might be expected for veneered zirconia and PFM restorations, in spite of the large difference in substrate hardness. Differences in susceptibility to chip spalling were not detected, but the chips in both specimen types detached off the sides in a similar manner instead of extending into the substrates.

Fracture strength of silicon carbide microspecimens

Polycrystalline silicon carbide tensile microspecimens 3.1 mm long were produced by deep reactive ion etching of wafers on the order of 150 /spl mu/m thick. The gage sections, which were nominally 200 /spl mu/m wide, were either straight, slightly curved, or contained double notches in order to vary the size of the highly stressed region. The fracture stresses of 190 specimens from three process runs were measured in a novel test setup. The average local fracture strengths for the last run were: straight 0.38/spl plusmn/0.13 GPa, curved 0.47/spl plusmn/0.15 GPa, notched 0.78/spl plusmn/0.28 GPa. The corresponding Weibull characteristic strengths were, 0.42 GPa, 0.53GPa, and 0.88 GPa with respective moduli 3.3, 3.4, and 3.1. These results show a clear increase in the strength of the material as the size of the highly stressed region decreases. Fractographic analyzes showed failures initiating from the bottoms of side grooves left by the etching process. The grains of the material were quite heterogeneous, varying from a few microns in size to columnar grains through the entire specimen thickness. The curved specimens were used as the base for predicting the probability of failure of the other two shapes. While the Weibull approach was quite accurate for the straight shape, it over-predicted the strengths of the notched specimens. Given the microstructure of the material relative to the size of the specimen, a continuum analysis is questionable.

ON THE NATURE OF MACHINING CRACKS IN GROUND CERAMICS: PART I: SRBSN STRENGTHS AND FRACTOGRAPHIC ANALYSIS

ABSTRACT Machining cracks in ground sintered reaction-bonded silicon nitride (SRBSN) rods and bars were analyzed by fractographic techniques. Grinding flaw sizes were as small as 12 µm and as large as 80 µm and correlated strongly with grinding direction and wheel grit size. Some grinding treatments had no deleterious effect on strength since the machining cracks were very small and fracture occurred from the materials inherent flaws. The telltale signs of machining damage may be detected with conventional low power optical microscopy using simple fractographic techniques. The telltale signs are summarized in a new series of schematic drawings which will aid pattern recognition for engineers and fractographers.