Integration Concepts for the Fabrication of LTCC Structures

At the Keck Smart Materials Integration Laboratory at Penn State University, low-temperature co-fired ceramic (LTCC) material systems have been used to fabricate a number of devices for a variety of applications. This article presents an overview of the integration of the concepts and materials that we have used to achieve miniaturization and unique device function. Examples of microwave filters, metamaterial antennas, and a dielectrophoretic cell sorter will be presented, with emphasis on device modeling and design, prototype construction methods, and test results.     

Kinetics of crack healing and self-repair behaviors in a sealant glass for SOFC applications

A sealant is required for the solid oxide fuel cell (SOFC) to maintain hermeticity at high operating temperatures, keep fuel and oxidant from mixing, and avoid shorting of the cell stack. Glass and glass–ceramic materials are widely used as a sealant because their properties can be tailored to meet the stringent requirements of SOFC stack, but they are susceptible to cracking. In contrast, a promising concept of self-repairable glass for seals is pursued for making reliable seals that can self-repair cracks at the SOFC operating temperatures. This concept is studied through measuring crack-healing kinetics and independent measurement of glass viscosity for relating to the observed self-repair. The cracks on the glass surface are created using a Vickers indenter to achieve a well-defined crack geometry, and then the glass is exposed to elevated temperatures for different length of times to study the crack-healing kinetics. The crack-healing kinetics is compared with the predictions of our theoretical model and found to be in good agreement. In addition, glass viscosity is extracted from the healing kinetics and compared with the independent measurement of viscosity measured from the dilatometry and sintering data to further validate the crack-healing theoretical model. These results are presented and discussed.     

The Change of X‐ray Diffraction Peak Width During in situ Conventional Sintering of Nanoscale Powders

Diffraction peaks of nanoscale particles of 3 mol% yttria‐stabilized zirconia become sharper as the powder sinters. The reduction in the peak width is correlated with the increase in density. The sharpening of the peak agrees reasonably well with the remaining free surface area as the sample sinters. Therefore, high curvature of the free surface of the pores is assumed to lead to peak broadening (the grain boundaries that grow at the expense of the free surfaces of the pores do not have this curvature). The change in the grain size during sintering does not make a significant contribution to peak width.     

rGO Sheets/ZnFe2O4 Nanocomposities as an Efficient Electro Catalyst Material for I3−/I− Reaction for High Performance DSSCs

In this paper, Reduced Graphene Oxide (rGO)/ZnFe₂O₄ (rZnF) nanocomposite is synthesized by a simple hydrothermal method and employed as a counter electrode (CE) material for tri-iodide redox reactions in Dye sensitized solar cells (DSSC) to replace the traditional high cost platinum (Pt) CE. X-ray diffraction analysis and High resolution Transmission electron microscopy, clearly indicated the formation of rZnF nanocomposite and also amorphous rGO sheets were smoothly distributed on the surface of ZnFe₂O₄ (ZnF) nanostructure. The rZnF-50 CE shows excellent electro catalytic activity toward I₃^? reduction, which has simultaneously been confirmed by cyclic voltammetry, electrochemical impedance spectroscopy and Tafel polarization measurements. A DSSC developed by rZnF-50 CE (η?=?8.71%) obtained quite higher than the Pt (η?=?8.53%) based CE under the same condition. The superior performances of rZnF-50 CE due to addition of graphene in to Spinel (ZnF) nanostructure results in creation of highly active electrochemical sites, fast electron transport linkage between CE and electrolyte. Thus it’s a promising low cost CE material for DSSCs.

     

Field assisted and flash sintering of alumina and its relationship to conductivity and MgO-doping

We show that flash-sintering in MgO-doped alumina is accompanied by a sharp increase in electrical conductivity. Experiments that measure conductivity in fully dense specimens, prepared by conventional sintering, prove that this is not a cause-and-effect relationship, but instead that the concomitant increase in the sintering rate and the conductivity share a common mechanism. The underlying mechanism, however, is mystifying since electrical conductivity is controlled by the transport of the fastest moving charged species, while sintering, which requires molecular transport or chemical diffusion, is limited by the slow moving charged species. Joule heating of the specimen during flash sintering cannot account for the anomalously high sintering rates. The sintering behavior of MgO-doped alumina is compared to that of nominally pure-alumina: the differences provide insight into the underlying mechanism for flash-sintering. We show that the pre-exponential in the Arrhenius equation for conductivity is enhanced in the non-linear regime, while the activation energy remains unchanged. The nucleation of Frenkel pairs is proposed as a mechanism to explain the coupling between flash-sintering and the non-linear increase in the conductivity.     

Transient analysis of a gas manifold system

In the present work, a numerical study has been carried out to predict transient gas flow and pressure behaviour in a gas manifold system. The start‐up and shutdown of the system, varying demands at the consumer ends, malfunctioning of compressors and valves are a few examples of common causes of transience in a gas delivery system. In particular, the sensitivity of oscillations in pressure and mass flux to variation in pipe dimensions, supply pressure and gas flow rate are ascertained under the aforementioned conditions of transience. The present results show that large pipe dimensions, high gas flow rate and high upstream pressure in the branch in which the disturbance is introduced, all cause greater amplitude in mass flux and pressure oscillations in the neighboring branches. The duration of oscillations is also found to be longer. The present study has practical importance in designing as well as in operating, a gas delivery system.     

Studies of spinodal decomposition in a ternary polymer‐solvent‐nonsolvent system

Much of the work in modeling and computer simulation of spinodal decomposition has been done for binary systems. This work attempts to carry out the analysis of spinodal decomposition in ternary polymer‐solvent‐nonsolvent systems, where the solvent is the monomer used to produce the polymer and the nonsolvent is the major component. Various experimental methods are used to determine values of the parameters of the ternary version of the Cahn‐Hilliard equation of spinodal decomposition, such as cloudpoint experiments, time‐resolved light scattering in the ternary system, and morphological development of polymer membranes formed during the early stages spinodal decomposition. The combination of these experimental methods and computer simulation work shows the validity of the assumptions made in characterizing spinodal decomposition in ternary polymer systems of interest.     

Crystallization of Polymer-Derived Silicon Carbonitride at 1873 K under Nitrogen Overpressure

The chemical stability of an amorphous silicon carbonitride ceramic, having the composition 0.57SiC·0.43Si₃N₄·0.49C is studied as a function of nitrogen overpressure at 1873 K. The ceramic suffers a weight loss at p _N2 < 3.5 bar (1 bar = 100 kPa), does not show a weight change from 3.5 to 11 bar, and gains weight above 11 bar. The structure of the ceramic changes with pressure: it is crystalline from 1 to 6 bar, amorphous at ∼10 bar, and is crystalline above ∼10 bar. The weight-loss transition, at 3.5 bar, is in excellent agreement with the prediction from thermodynamic analysis when the activities of carbon, SiC, and Si₃N₄ are set equal to those of the crystalline forms; this implies that the material crystallizes before decomposition. The amorphous to crystalline transition that occurs at ∼10 bar, and which is accompanied by weight gain, is likely to have taken place by a different mechanism. A nucleation and growth reaction with the atmospheric nitrogen is proposed as the likely mechanism. The supersaturation required to nucleate α-Si₃N₄ crystals is calculated to be 30 kJ/mol.     

Solid Yttria-Stabilized Zirconia Films by Pulsed Chemical Vapor Deposition from Metal-organic Precursors

A pulsed chemical vapor deposition from metal-organic precursors (MOCVD) system was used to produce solid zirconia, and yttria-stabilized zirconia (YSZ) films. A total of six candidate metal-organic precursors for zirconia and three for yttria were investigated. Three precursor solutions for YSZ proved suitable for pulsed-MOCVD processing. Layers were deposited on metal, alumina, and porous nickel cermet substrates. Under optimal deposition conditions, precursor conversion efficiency of 90% was achieved using a solution of 3.74 vol% zirconium 2-methyl-2-butoxide + 0.42% yttium methoxyethoxide in toluene. The film growth rate was 7.5 μm·h⁻¹ at 525°C deposition temperature. Two alkoxide precursors produced YSZ layers with material costs under $0.50/(μm·cm²).     

Mechanically robust and thermally enhanced sand-polyacrylamide-2D nanofiller composite hydrogels for water shutoff applications

Herein, we report a facile preparation method for mechanically robust and thermally enhanced sand-polyacrylamide (PAM)-2D-nanofillers composite hydrogels and their application in water shutoff. To prepare the sample, 4 wt% of aqueous PAM solution is mixed with organic cross-linkers of hydroquinone (HQ) and hexamethylenetetramine (HMT) in a 1:1 weight ratio and aqueous potassium chloride (KCl) solution and with a specific amount of 2D-nanofillers such as commercial graphene (CG) nanosheets or boron nitride nanoparticles (BN NPs). A specific amount of the above solution is added to sand, well mixed, and subsequently cured at 150°C for 8 h. The prepared composite hydrogels were characterized by Fourier-transform infrared spectroscopy (FT-IR) for chemical composition and X-ray diffraction (XRD) for successful hydrogel coating onto the sand particles. Thermal stabilities of the samples have been evaluated by differential scanning calorimetry (DSC). Mechanical properties (storage modulus [G′]; loss modulus [G″]; gel strength (G′/G″); and damping factor [G″/G′]) of the samples were determined using dynamic mechanical analyses. The thermal stability of the samples has reached as high as 193.4°C, while the gel strength is found to be a maximum of 16.2. The water swelling ratio for the composite hydrogel has reached a maximum of 1100% within 1 h.