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Pressure-Induced Phase Transformation of Controlled-Porosity Pb(Zr0.95Ti0.05)O3 Ceramics

Journal of the American Ceramic Society

Tuttle, Bruce T.; Yang, Pin Y.; Gieske, John H.; Voigt, James A.; Scofield, Timothy W.; Zeuch, David H.; Olson, Walter R.

Chemically prepared Pb(Zr0.95Ti0.05)O3 (PZT 95/5) ceramics were fabricated with a range of different porosity levels, while grain size was held constant, by systematic additions of added organic pore former (Avicel). Use of Avicel in amounts ranging from 0 to 4.0 wt% resulted in fired ceramic densities that ranged from 97.3% to 82.3%. Hydrostatic-pressure-induced ferroelectric (FE) to antiferroelectric (AFE) phase transformations were substantially more diffuse and occurred at lower hydrostatic pressures with increasing porosity. An ∼12 MPa decrease in hydrostatic transformation pressure per volume percent added porosity was observed. The decrease in transformation pressure with decreasing density was quantitatively consistent with the calculated macroscopic stress required to achieve a specific volumetric macrostrain (0.40%). This strain was equivalent to experimentally measured macrostrain for FE-to-AFE transformation. The macroscopic stress levels were calculated using measured bulk modulus values that decreased from 84 to 46 GPa as density decreased from 97.3% to 82.3%. Good agreement between calculated and measured values of FE-to-AFE transformation stress was obtained for ceramics fired at 1275° and 1345°C.

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Raman Spectroscopic and Ultrasonic Measurements to Monitor the HMX ( ) Phase Transition

Tappan, Alexander S.; Renlund, Anita M.; Gieske, John H.; Miller, Jill C.

The HMX {beta}-{delta} solid-solid phase transition, which occurs as HMX is heated near 170 C, is clearly linked to increased reactivity and sensitivity to initiation. Thermally damaged energetic materials (EMs) containing HMX therefore may present a safety concern. Information about the phase transition is vital to a predictive safety model for HMX and HMX-containing EMs. We report work in progress on monitoring the phase transition with real-time Raman spectroscopy and ultrasonic measurements aimed towards a better understanding of physical properties through the phase transition. HMX samples were confined with minimal free volume.in a cell with constant volume. The cell was heated at a controlled rate and real-time Raman spectroscopic or ultrasonic measurements were performed. Raman spectroscopy provides a clear distinction between the two phases because the vibrational transitions of the molecule change with confirmational changes associated with the phase transition. Ultrasonic time-of-flight measurements provide an additional method of distinguishing the two phases because the sound speed through the material changes with the phase transition. Ultrasonic attenuation measurements also provide information about microstructural changes such as increased porosity due to evolution of gaseous decomposition products.

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Ultrasonic inspection technique for composite doubler/aluminum skin bond integrity for aircraft

Proceedings of SPIE - The International Society for Optical Engineering

Gieske, John H.

As part of the FAA's National Aging Aircraft Research Program to foster new technologies for civil aircraft maintenance and repair, use of bonded composite doublers on metal aircraft structures has been advanced. Research and validation of such doubler applications on U.S. certified commercial aircraft has begun. A specific composite application to assess the capabilities of composite doublers was chosen on a L-1011 aircraft for reinforcement of the corner of a cargo door frame where a boron-epoxy repair patch of up to 72 plies was installed. A primary inspection requirement for these doublers is the identification of disbonds between the composite laminate and the aluminum parent material. This paper describes the development of an ultrasonic pulse-echo technique using a modified immersion focus transducer where a robust signal amplitude signature of the composite/aluminum interface is obtained to characterize the condition of the bond. Example waveforms and C-scan images are shown to illustrate the ultrasonic response for various transducer configurations using a boron-epoxy/aluminum skin calibration test sample where disbonds and delaminations were built-in. The modified focus transducer is compatible with portable ultrasonic scanning systems that utilize the weeper or dripless bubbler technologies when an ultrasonic inspection of the boron-epoxy composite doublers installed on aircraft is implemented.

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Nondestructive evaluation (NDE) of composite-to-metal bond interface of a wind turbine blade using an acousto-ultrasonic technique

Gieske, John H.

An acousto-ultrasonic inspection technique was developed to evaluate the structural integrity of the epoxy bond interface between a metal insert and the fiber glass epoxy composite of a wind turbine blade. Data was generated manually as well as with a PC based data acquisition and display system. C-scan imaging using a portable ultrasonic scanning system provided an area mapping of the delamination or disbond due to fatigue testing and normal field operation conditions of the turbine blade. Comparison of the inspection data with a destructive visual examination of the bond interface to determine the extent of the disbond showed good agreement between the acousto-ultrasonic inspection data and the visual data.

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Evaluation of scanners for C-scan imaging in nondestructive inspection of aircraft

Gieske, John H.

The goal of this project was to produce a document that contains information on the usability and performance of commercially available, fieldable, and portable scanner systems as they apply to aircraft NDI inspections. In particular, the scanners are used to generate images of eddy current, ultrasonic, or bond tester inspection data. The scanner designs include manual scanners, semiautomated scanners, and fully automated scanners. A brief description of the functionality of each scanner type, a sketch, and a fist of the companies that support the particular design are provided. Vendors of each scanner type provided hands-on demonstrations of their equipment on real aircraft samples in the FAA Aging Aircraft Nondestructive Inspection Validation Center (AANC) in Albuquerque, NM. From evaluations recorded during the demonstrations, a matrix of scanner features and factors and ranking of the capabilities and limitations of the design, portability, articulation, performance, usability, and computer hardware/software was constructed to provide a quick reference for comparing the different scanner types. Illustrations of C-scan images obtained during the demonstration are shown.

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Development of ultrathin, dimensionally stable composites for the Superconducting Super Collider (SSC) elementary particle detectors

Gieske, John H.

The Los Alamos National Laboratory (LANL) Mechanical Engineering and Electronics Division, in partnership with Sandia National Laboratories and Programmed Composites, is advancing the development of thin-walled, high modulus short-fiber compression-molded composite materials fabrication. In this paper, we investigate component uniformity, structural integrity, thermal conductivity, and radiation resistance; discuss the scanning-electron microscopic inspection of the graphite fiber distribution and orientation, and describe the process used in selecting the reinforcement fiber length and modulus and for choosing the hydrophobic, cyanate-ester resin.

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7 Results
7 Results