Marina R. Pascucci

Active PZT fibers: a commercial production process

Lead Zirconate Titanate (PZT) active fibers, from 80 to 250 micrometers in diameter, are produced for the AFOSR/DARPA funded Active Fiber Composites Consortium (AFCC) Program and commercial customers. CeraNova has developed a proprietary ceramics-based technology to produce PZT mono-filaments of the required purity, composition, straightness, and piezoelectric properties for use in active fiber composite structures. CeraNovas process begins with the extrusion of continuous lengths of mono-filament precursor fiber from a plasticized mix of PZT-5A powder. The care that must be taken to avoid mix contamination is described using illustrations form problems experiences with extruder wear and metallic contamination. Corrective actions are described and example microstructures are shown. The consequences of inadequate lead control are also shown. Sintered mono- filament mechanical strength and piezoelectric properties data approach bulk values but the validity of such a benchmark is questioned based on variable correlation with composite performance measures. Comb-like ceramic preform structures are shown that are being developed to minimize process and handling costs while maintaining the required mono-filament straightness necessary for composite fabrication. Lastly, actuation performance data are presented for composite structures fabricated and tested by Continuum Control Corporation. Free strain actuation in excess of 2000 microstrain are observed.

Transparent ceramics for sensor applications

Transparent ceramics are finding applications in demanding optical applications were traditional mineral salts and amorphous materials are limited and single crystals are not practical. Polycrystalline ceramics offer a unique combination of mechanical, electrical and optical properties that allow window and dome applications and possibilities that were previously not possible. Transparent ceramics are being developed for use in a number of applications with each material possessing a distinctive set of properties that address a particular application. The current status of CeraNova’s fine grain transparent ceramic programs for dome and window applications will be presented with emphasis on their exceptional material properties for specific applications.

Polycrystalline alumina for aerodynamic IR domes and windows

CeraNovas transparent polycrystalline alumina (CeraLuminTM)a has sub-micron grain size (300-500nm) and high transmittance in the mid-wave infrared (>85% in the 3-5µm MWIR region). The fine, uniform grain size imparts high hardness, high strength, and high thermal shock resistance. Polycrystalline alumina is a viable alternative to sapphire for domes, particularly for aerodynamic shapes which are readily fabricated by powder processing. Both hemispheric and ogive domes (sub-scale and full-size) have been successfully molded and densified to transparency. Hemispheric domes have been optically finished. Current efforts include a focus on scale-up, fabrication, and metrology of aerodynamic domes. This paper presents recent analyses of microstructure, optical properties, and mechanical properties.

Transparent ceramics for demanding optical applications

Transparent ceramics are finding applications is demanding optical applications were traditional mineral salts and amorphous materials are limited and single crystals are not practical. Polycrystalline ceramics offer a unique combination of mechanical, electrical and optical properties that allow window and dome applications and possibilities that were previously not possible. Transparent ceramics are being developed for use in a number of applications with each material possessing a distinctive set of properties that address a particular application. The current status of CeraNovas fine grain transparent ceramic programs for dome and window applications will be presented with emphasis on their exceptional properties for specific applications.

Extruded electroactive fibers: preferred crystallographic orientation

Electroactive fibers of preferred macro crystalline orientation and ultimately single crystal structure are goals of the research discussed in this paper. Four compositions are under evaluation; lead magnesium niobate- lead titanate solid solution, PMN-31PT, an incongruently melting near-morphotropic phase boundary piezoelectric composition; PMN-10PT, an electrostrictor composition; and two lead free compositions in the sodium bismuth titanate- barium titanate solid solution, NbiT-BaT, family, both congruently melting, one electrostrictor and one piezoelectric. The efficacy of seed crystals in stimulating oriented crystal growth is being evaluated in the lead-based PMN-31PT system. Sub-micron reactive precursor powders of high chemical potential are being evaluated as matrix material. Direct fiber and ribbon extrusion have been shown to orient high chemical potential are being evaluated as matrix material. Direct fiber and ribbon extrusion have been shown to orient high chemical potential are being evaluated as matrix material. Direct fiber and ribbon extrusion have been shown to orient prismatic, needle and platelet shaped seed crystals. Extrusion orifice, seed and initial matrix particle size have not influenced the degree of seed orientation within the tested bounds of our experimental parameters. Non-equilibrium sintering conditions near the melting points of all four compositions noted above will be used to generate exaggerated grain growth under seeded and self-seeding conditions. In the PMN-31PT system, an as yet uncharacterized melt phase appears to stimulate rapid crystal growth, the orientation of which shall be determined by x-ray back reflection Laue methods. Analyses of fiber composition and grain orientation are ongoing. Results to-date will be reported. Analyses of fiber quality and performance, measured using single fiber P-E loop testing, are presented. Loops of sufficient quality to warrant fiber evaluation in active fiber composite packs have been measured. Progress toward program goals is summarized in this paper.

Strength characteristics of transparent alumina and spinel ceramics

Transparent ceramics are finding increasing use in optical applications with demanding operating conditions. Polycrystalline ceramics provide a unique combination of mechanical, dielectric and optical properties for sensor window applications that were previously not possible. The mechanical strength of CeraNova’s transparent alumina and spinel was measured by an equibiaxial strength test method. The results of the tests and their analysis, included those at elevated temperatures for transparent alumina, will be presented.

Refractive index of infrared-transparent polycrystalline alumina

The refractive index of polycrystalline α-alumina prisms with an average grain size of 0.6 μm is reported for the wavelength range 0.9 to 5.0 and the temperature range 293 to 498K. Results agree within 0.0002 with the refractive index predicted for randomly oriented grains of single-crystal aluminum oxide. This paper provides tutorial background on the behavior of birefringent materials and explains how the refractive index of polycrystalline alumina can be predicted from the ordinary and extraordinary refractive indices of sapphire. The refractive index of polycrystalline alumina is described by 𝑛𝑛2 − 1 = (A+B [𝑇𝑇2−𝑇𝑇20]) +Dλ2 /λ2−(λ1+C [𝑇𝑇2−𝑇𝑇20])2 + λ2−λ22 where wavelength λ is expressed in μm, To = 295.15 K, A = 2.07156, B = 6.273× 10-8, λ1 = 0.091293, C = –1.9516 × 10-8, D = 5.62675, and λ2 = 18.5533. The slope dn/dT varies with λ and T, but has the approximate value 1.4 × 10-5 K-1 in the range 296–498 K.

Slow crack growth study of polycrystalline alumina and multispectral zinc sulfide

Samples of fine-grain, transparent polycrystalline alumina (CeraNova Corp) and multispectral zinc sulfide (Cleartran) were tested to determine mechanical strength and slow crack growth parameters. Mechanical strength measurements of coupons were fit to a Weibull equation that describes the material strength and its distribution. Slow crack growth parameters were calculated using the procedure set forth by Weiderhorn.1 This paper describes the derivation of Weibull and slow crack growth parameters from strength measurements over a range of stress rates and how these parameters are used to predict window lifetime under stress. Proof testing is employed to ensure that a window begins its life with a known, minimum strength.