Compositional homogeneity of ferroelectric (Pb,La)(Ti,Zr)O3 thick films

2003 ◽  
Vol 18 (2) ◽  
pp. 515-523 ◽  
Author(s):  
S. Bernik ◽  
R.B. Marinenko ◽  
J. Holc ◽  
Z. Samardžija ◽  
M. Čeh ◽  
...  

Quantified wavelength dispersive spectroscopy (WDS) x-ray element maps were used to characterize active (Pb,La)(Ti,Zr)O3 (PLZT) layers on Pt/PLZT/Al2O3 substrates, one fired at 1050 °C and the other at 1150 °C. In the layer fired at 1050 °C, randomly distributed micrometer-sized compositional irregularities were observed as La-rich regions that were in most cases enriched also with Ti and deficient in Pb and Zr compared to the matrix. Such compositional imperfections were not observed in the PLZT layer fired for the same duration at 1150 °C. The level of microheterogeneity for all elements in the specimen fired at 1150 °C and for Pb, Ti, and Zr in the specimen fired at 1050 °C was below 1% relative at confidence level of 99% while for La it was as much as 2.5% relative. In point-beam line profiles across the active layer starting from the Pt electrode toward the outer surface of the cross-section of the PLZT film, the Pb concentration decreased continuously in both samples, confirming the importance of providing a properly equilibrated partial pressure of Pb around the sample during the entire firing process. Better dielectric and ferroelectric characteristics of the specimen fired at 1150 °C compared to the sample fired at 1050 °C were attributed to the differences in compositional heterogeneity between these samples. The study of the micro-compositional characteristics of these ceramic materials with quantitative WDS mapping has contributed to the optimization of processing parameters and hence to the understanding of the properties of ferroelectric PLZT materials.

Author(s):  
H.J. Dudek

The chemical inhomogenities in modern materials such as fibers, phases and inclusions, often have diameters in the region of one micrometer. Using electron microbeam analysis for the determination of the element concentrations one has to know the smallest possible diameter of such regions for a given accuracy of the quantitative analysis.In th is paper the correction procedure for the quantitative electron microbeam analysis is extended to a spacial problem to determine the smallest possible measurements of a cylindrical particle P of high D (depth resolution) and diameter L (lateral resolution) embeded in a matrix M and which has to be analysed quantitative with the accuracy q. The mathematical accounts lead to the following form of the characteristic x-ray intens ity of the element i of a particle P embeded in the matrix M in relation to the intensity of a standard S


Author(s):  
J.Y. Laval

The exsolution of magnetite from a substituted Yttrium Iron Garnet, containing an iron excess may lead to a transitional event. This event is characterized hy the formation of a transitional zone at the center of which the magnetite nucleates (Fig.1). Since there is a contrast between the matrix and these zones and since selected area diffraction does not show any difference between those zones and the matrix in the reciprocal lattice, it is of interest to analyze the structure of the transitional zones.By using simultaneously different techniques in electron microscopy, (oscillating crystal method microdiffraction and X-ray microanalysis)one may resolve the ionic process corresponding to the transitional event and image this event subsequently by high resolution technique.


Author(s):  
C.M. Sung ◽  
K.J. Ostreicher ◽  
M.L. Huckabee ◽  
S.T. Buljan

A series of binary oxides and SiC whisker reinforced composites both having a matrix composed of an α-(Al, R)2O3 solid solution (R: rare earth) have been studied by analytical electron microscopy (AEM). The mechanical properties of the composites as well as crystal structure, composition, and defects of both second phases and the matrix were investigated. The formation of various second phases, e.g. garnet, β-Alumina, or perovskite structures in the binary Al2O3-R2O3 and the ternary Al2O3-R2O3-SiC(w) systems are discussed.Sections of the materials having thicknesses of 100 μm - 300 μm were first diamond core drilled. The discs were then polished and dimpled. The final step was ion milling with Ar+ until breakthrough occurred. Samples prepared in this manner were then analyzed using the Philips EM400T AEM. The low-Z energy dispersive X-ray spectroscopy (EDXS) data were obtained and correlated with convergent beam electron diffraction (CBED) patterns to identify phase compositions and structures. The following EDXS parameters were maintained in the analyzed areas: accelerating voltage of 120 keV, sample tilt of 12° and 20% dead time.


Author(s):  
Edgar S. Etz ◽  
Thomas D. Schroeder ◽  
Winnie Wong-Ng

We are investigating by Raman microprobe measurements the superconducting and related phases in the LnBa2Cu3O7-x (for x=0 to 1) system where yttrium has been replaced by several of the lanthanide (Ln = Nd,Sm,Eu,Ho,Er) elements. The aim is to relate the observed optical spectra (Raman and fluorescence) to the compositional and structural properties of these solids as part of comprehensive materials characterization. The results are correlated with the methods of synthesis, the processing techniques of these materials, and their superconducting properties. Of relevance is the substitutional chemistry of these isostructural systems, the differences in the spectra, and their microanalytical usefulness for the detection of impurity phases, and the assessment of compositional homogeneity. The Raman spectra of most of these compounds are well understood from accounts in the literature.The materials examined here are mostly ceramic powders prepared by conventional solid state reaction techniques. The bulk samples are of nominally single-phase composition as determined by x-ray diffraction.


Author(s):  
Richard B. Mott ◽  
John J. Friel ◽  
Charles G. Waldman

X-rays are emitted from a relatively large volume in bulk samples, limiting the smallest features which are visible in X-ray maps. Beam spreading also hampers attempts to make geometric measurements of features based on their boundaries in X-ray maps. This has prompted recent interest in using low voltages, and consequently mapping L or M lines, in order to minimize the blurring of the maps.An alternative strategy draws on the extensive work in image restoration (deblurring) developed in space science and astronomy since the 1960s. A recent example is the restoration of images from the Hubble Space Telescope prior to its new optics. Extensive literature exists on the theory of image restoration. The simplest case and its correspondence with X-ray mapping parameters is shown in Figures 1 and 2.Using pixels much smaller than the X-ray volume, a small object of differing composition from the matrix generates a broad, low response. This shape corresponds to the point spread function (PSF). The observed X-ray map can be modeled as an “ideal” map, with an X-ray volume of zero, convolved with the PSF. Figure 2a shows the 1-dimensional case of a line profile across a thin layer. Figure 2b shows an idealized noise-free profile which is then convolved with the PSF to give the blurred profile of Figure 2c.


1986 ◽  
Vol 47 (C8) ◽  
pp. C8-135-C8-137
Author(s):  
T. MURATA ◽  
T. MATSUKAWA ◽  
M. MORI ◽  
M. OBASHI ◽  
S.-I. NAO-E ◽  
...  

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Avanish Mishra ◽  
Cody Kunka ◽  
Marco J. Echeverria ◽  
Rémi Dingreville ◽  
Avinash M. Dongare

AbstractDuring the various stages of shock loading, many transient modes of deformation can activate and deactivate to affect the final state of a material. In order to fundamentally understand and optimize a shock response, researchers seek the ability to probe these modes in real-time and measure the microstructural evolutions with nanoscale resolution. Neither post-mortem analysis on recovered samples nor continuum-based methods during shock testing meet both requirements. High-speed diffraction offers a solution, but the interpretation of diffractograms suffers numerous debates and uncertainties. By atomistically simulating the shock, X-ray diffraction, and electron diffraction of three representative BCC and FCC metallic systems, we systematically isolated the characteristic fingerprints of salient deformation modes, such as dislocation slip (stacking faults), deformation twinning, and phase transformation as observed in experimental diffractograms. This study demonstrates how to use simulated diffractograms to connect the contributions from concurrent deformation modes to the evolutions of both 1D line profiles and 2D patterns for diffractograms from single crystals. Harnessing these fingerprints alongside information on local pressures and plasticity contributions facilitate the interpretation of shock experiments with cutting-edge resolution in both space and time.


Coatings ◽  
2021 ◽  
Vol 11 (1) ◽  
pp. 105
Author(s):  
Seung Hyun Park ◽  
Kyung Eon Kim ◽  
Sang Jeen Hong

Coating the inner surfaces of high-powered plasma processing equipment has become crucial for reducing maintenance costs, process drift, and contaminants. The conventionally preferred alumina (Al2O3) coating has been replaced with yttria (Y2O3) due to the long-standing endurance achieved by fluorine-based etching; however, the continuous increase in radio frequency (RF) power necessitates the use of alternative coating materials to reduce process shift in a series of high-powered semiconductor manufacturing environments. In this study, we investigated the fluorine-based etching resistance of atmospheric pressure-sprayed alumina, yttria, yttrium aluminum garnet (YAG), and yttrium oxyfluoride (YOF). The prepared ceramic-coated samples were directly exposed to silicon oxide etching, and the surfaces of the plasma-exposed samples were characterized by scanning electron microscopy, energy-dispersive X-ray spectroscopy, and X-ray photoelectron spectroscopy. We found that an ideal coating material must demonstrate high plasma-induced structure distortion by the fluorine atom from the radical. For endurance to fluorine-based plasma exposure, the bonding structure with fluoride was shown to be more effective than oxide-based ceramics. Thus, fluoride-based ceramic materials can be promising candidates for chamber coating materials.


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