NDE reliability and process control for structural ceramics

The reliability of microfocus x-radiography and scanning laser acoustic microscopy for detecting microvoids in silicon nitride and silicon carbide was statistically evaluated. Materials- and process-related parameters that influenced the statistical findings in research samples are discussed. The use of conventional x-radiography in controlling and optimizing the processing and sintering of an Si3N4-Si02-Y203 composition designated NASA 6Y is described. Radiographic evaluation and guidance helped develop uniform high-density Si3N4 modulus-of-rupture bars with improved four-point flexural strength (857, 544, and 462 MPa at room temperature, 1200 C, and 1370 C, respectively) and reduced strength scatter

Ultrasonic characterization of structural ceramics

Ultrasonic velocity and attenuation measurements were used to characterize density and microstructure in monolithic silicon nitride and silicon carbide. Research samples of these structural ceramics exhibited a wide range of density and microstructural variations. It was shown that bulk density variations correlate with and can be estimated by velocity measurements. Variations in microstructural features such as grain size or shape and pore morphology had a minor effect on velocity. However, these features had a pronounced effect on ultrasonic attenuation. The ultrasonic results are supplemented by low-energy radiography and scanning laser acoustic microscopy

Effect of stress on ultrasonic pulses in fiber reinforced composites

An acoustical-ultrasonic technique was used to demonstrate relationships existing between changes in attenuation of stress waves and tensile stress on an eight ply 0 degree graphite-epoxy fiber reinforced composite. All tests were conducted in the linear range of the material for which no mechanical or macroscopic damage was evident. Changes in attenuation were measured as a function of tensile stress in the frequency domain and in the time domain. Stress wave propagation in these specimens was dispersive, i.e., the wave speed depends on frequency. Wave speeds varied from 267,400 cm/sec to 680,000 cm/sec as the frequency of the signal was varied from 150 kHz to 1.9 MHz which strongly suggests that flexural/lamb wave modes of propagation exist. The magnitude of the attenuation changes depended strongly on tensile stress. It was further observed that the wave speeds increased slightly for all tested frequencies as the stress was increased

Probability of detection of internal voids in structural ceramics using microfocus radiography

The reliability of microfocus x-radiography for detecting subsurface voids in structural ceramic test specimens was statistically evaluated. The microfocus system was operated in the projection mode using low X-ray photon energies (20 keV) and a 10 micro m focal spot. The statistics were developed for implanted subsurface voids in green and sintered silicon carbide and silicon nitride test specimens. These statistics were compared with previously-obtained statistics for implanted surface voids in similar specimens. Problems associated with void implantation are discussed. Statistical results are given as probability-of-detection curves at a 95 percent confidence level for voids ranging in size from 20 to 528 micro m in diameter

Correlation of processing and sintering variables with the strength and radiography of silicon nitride

A sintered Si3N4-SiO2-Y2O3 composition, NASA 6Y, was developed that reached four-point flexural average strength/standard deviation values of 857/36, 544/33, and 462/59 MPa at room temperature, 1200 and 1370 C respectively. These strengths represented improvements of 56, 38, and 21 percent over baseline properties at the three test temperatures. At room temperature the standard deviation was reduced by over a factor of three. These accomplishments were realized by the iterative utilization of conventional x-radiography to characterize structural (density) uniformity as affected by systematic changes in powder processing and sintering parameters. Accompanying the improvement in mechanical properties was a change in the type of flaw causing failure from a pore to a large columnar beta- Si3N4 grain typically 40 to 80 microns long, 10 to 30 microns wide, and with an aspect ratio of 5:1

Radiographic detectability limits for seeded voids in sintered silicon carbide and silicon nitride

Conventional and microfocus X-radiographic techniques were compared to determine relative detectability limits for voids in green and sintered SiC and Si3N4. The relative sensitivity of the techniques was evaluated by comparing their ability to detect voids that were artificially introduced by a seeding process. For projection microfocus radiography the sensitivity of void detection at a 90/95 probability of detection/confidence level is 1.5% of specimen thickness in sintered SiC and Si3N4. For conventional contact radiography the sensitivity is 2.5% of specimen thickness. It appears that microfocus projection radiography is preferable to conventional contact radiography in cases where increased sensitivity is required and where the additional complexity of the technique can be tolerated

The effect of stress on ultrasonic pulses in fiber reinforced composites

An acoustical-ultrasonic technique was used to demonstrate relationships existing between changes in attenuation of stress waves and tensile stress for an eight ply 0 degree graphite-epoxy fiber reinforced composite. All tests were conducted in the linear range of the material for which no mechanical or macroscopic damage was evident. Changes in attenuation were measured as a function of tensile stress in the frequency domain and in the time domain. Stress wave propagation in these specimens was dispersive, i.e., the wave speed depends on frequency. Wave speeds varied from 267 400 cm/sec to 680 000 cm/sec as the frequency of the signal was varied from 150 kHz to 1.9 MHz which strongly suggests that flexural/lamb wave modes of propagation exist. The magnitude of the attenuation changes depended strongly on tensile stress. It was further observed that the wave speeds increased slightly for all tested frequencies as the stress was increased

Reliability of scanning laser acoustic microscopy for detecting internal voids in structural ceramics

The reliability of 100 MHz scanning laser acoustic microscopy (SLAM) for detecting internal voids in sintered specimens of silicon nitride and silicon carbide was evaluated. The specimens contained artificially implanted voids and were positioned at depths ranging up to 2 mm below the specimen surface. Detection probability of 0.90 at a 0.95 confidence level was determined as a function of material, void diameter, and void depth. The statistical results presented for void detectability indicate some of the strengths and limitations of SLAM as a nondestructive evaluation technique for structural ceramics

Reliability of void detection in structural ceramics using scanning laser acoustic microscopy

The reliability of scanning laser acoustic microscopy (SLAM) for detecting surface voids in structural ceramic test specimens was statistically evaluated. Specimens of sintered silicon nitride and sintered silicon carbide, seeded with surface voids, were examined by SLAM at an ultrasonic frequency of 100 MHz in the as fired condition and after surface polishing. It was observed that polishing substantially increased void detectability. Voids as small as 100 micrometers in diameter were detected in polished specimens with 0.90 probability at a 0.95 confidence level. In addition, inspection times were reduced up to a factor of 10 after polishing. The applicability of the SLAM technique for detection of naturally occurring flaws of similar dimensions to the seeded voids is discussed. A FORTRAN program listing is given for calculating and plotting flaw detection statistics

Assessment of damage in ceramics and ceramic matrix composites using ultrasonic techniques

This paper addresses the application of ultrasonic sensing to damage assessment in ceramics and ceramic matrix composites. It focuses on damage caused by thermal shock or oxidation at elevated temperatures, which often results in elastic anisotropy. This damaged-induced anisotropy is determined by measuring the velocities of ultrasonic waves in different propagation directions. Thermal shock damage is assessed in ceramic samples of reaction bonded silicon nitride (RBSN). Thermal shock treatment from different temperatures up to 1000 C is applied to produce the microcracks. Results indicate that most microcracks produced by thermal shock are located near sample surfaces. Ultrasonic measurements using the surface wave method are found to correlate well with measurements of degradation of mechanical properties obtained independently by other authors using destructive methods. Oxidation damage is assessed in silicon carbide fiber/reaction bonded silicon nitride matrix (SCS-6/RBSN) composites. The oxidation is done by exposing the samples in a flowing oxygen environment at elevated temperatures, up to 1400 C, for 100 hr. The Youngs' modulus in the fiber direction as obtained from ultrasonic measurements decreases significantly at 600 C but retains its original value at temperatures above 1200 C. This agrees well with the results of destructive tests by other authors. On the other hand, the transverse moduli obtained from ultrasonic measurements decrease continually until 1200 C. Measurements on the shear stiffnesses show behavior similar to the transverse moduli. The results of this work show that the damage-induced anisotropy in both ceramics and ceramic matrix composites can be determined successfully by ultrasonic methods. This suggests the possibility of assessing damage severity using ultrasonic techniques