scholarly journals Stoichiometry and Interdiffusion in PZT Thin Films Studied by Transmission Electron Microscopy

1999 ◽  
Vol 596 ◽  
Author(s):  
L. Sagalowicz ◽  
P. Muralt ◽  
S. Hiboux ◽  
T. Maeder ◽  
K. Brooks ◽  
...  

AbstractElectrode stability, interdiffusion, phase purity and deviation from stoichiometry at the PZT-electrode interface are key issues in PZT thin film integration. This article highlights the use of transmission electron imaging combined with energy dispersive spectroscopy (EDS) for the investigation of these phenomena. The accuracy of the EDS analysis is discussed. It will be shown that using a standard PZT sample and controlled conditions, reliable analysis can be performed.Diffusion mechanisms have been studied for Pt based electrode systems and RuO2-based electrode systems developed for direct integration onto silicon. The materials studied were composed of stacks of silicon-silicon oxide, an adhesion layer (Ti, Ta or TiOx), an electrode (Pt or RuG2) and PZT (45/55). The PZT was deposited by sol gel using the same parameters to allow for comparison of the different electrodes. Four different electrode / adhesion layer materials were compared (Pt/Ti, Pt/TiOx, Pt/Ta and RuO2 / TiO2). In the case of Pt, lead and oxygen diffusion through the electrode is observed. While the initial Ta layer transforms into a homogeneous pyrochlore phase, the Ti adhesion layer is heavily deformed. In the case of TiOx the lead is mainly incorporated at the interfaces with Pt and with SiO2. No lead diffusion to the adhesion layer is observed for the RuO2 electrode. In-situ sputtering and sol-gel deposition of PZT are also compared. The sol-gel films are close to the right stoichiometry for the perovskite while the sputtered films contained an excess of lead. No sign of second phase is found by X-ray diffraction (XRD), by EDS and by high resolution transmission electron microscopy (HRTEM) which suggests that the excess lead is accommodated in the perovskite lattice.

2015 ◽  
Vol 2015 ◽  
pp. 1-8 ◽  
Author(s):  
Sanja Ćulubrk ◽  
Željka Antić ◽  
Vesna Lojpur ◽  
Milena Marinović-Cincović ◽  
Miroslav D. Dramićanin

Herein we presented hydrolytic sol-gel synthesis and photoluminescent properties of Eu3+-doped Gd2Ti2O7pyrochlore nanopowders. According to Gd2Ti2O7precursor gel thermal analysis a temperature of 840°C is identified for the formation of the crystalline pyrochlore phase. Obtained samples were systematically characterized by powder X-ray diffraction, scanning and transmission electron microscopy, and photoluminescence spectroscopy. The powders consist of well-crystalline cubic nanocrystallites of approximately 20 nm in size as evidenced from X-ray diffraction. The scanning and transmission electron microscopy shows that investigated Eu3+-doped Gd2Ti2O7nanopowders consist of compact, dense aggregates composed entirely of nanoparticles with variable both shape and dimension. The influence of Eu3+ions concentration on the optical properties, namely, photoluminescence emission and decay time, is measured and discussed. Emission intensity as a function of Eu3+ions concentration shows that Gd2Ti2O7host can accept Eu3+ions in concentrations up to 10 at.%. On the other hand, lifetime values are similar up to 3 at.% (~2.7 ms) and experience decrease at higher concentrations (2.4 ms for 10 at.% Eu3+). Moreover, photoluminescent spectra and lifetime values clearly revealed presence of structural defects in sol-gel derived materials proposing photoluminescent spectroscopy as a sensitive tool for monitoring structural changes in both steady state and lifetime domains.


2002 ◽  
Vol 17 (8) ◽  
pp. 2066-2074 ◽  
Author(s):  
Zhaoxia Zhou ◽  
Ian M. Reaney ◽  
David Hind ◽  
Steven J. Milne ◽  
Andy P. Brown ◽  
...  

Advanced analytical transmission electron microscopy has been used to investigate microstructural evolution during pyrolysis in triol-based sol-gel thin films. At pyrolysis temperatures up to 300 °C, the films remained amorphous; however, nanometer-sized precipitates were observed in films heat-treated up to 400 °C for 10 min. Analytical transmission electron microscopy indicated that the precipitates were Pb-rich, as well as deficient in O, Ti, and Zr. Films pyrolyzed up to 500 °C for 10 min were composed of a nanocrystalline pyrochlore phase; however, pores could be observed, situated in the same position as the nanometer-sized precipitates at 400 °C. Face-centered cubic Pb-rich crystallites were also present on the surface of pyrolyzed films but absent in the fully crystallized films annealed at 650 °C. A tentative mechanism is proposed to explain these observations.


1998 ◽  
Vol 13 (4) ◽  
pp. 974-978 ◽  
Author(s):  
Seong-Hyeon Hong ◽  
Naesung Lee ◽  
Altaf H. Carim ◽  
Gary L. Messing

Interfacial precipitation in sol-gel derived, titania-doped diphasic mullite gels was investigated using conventional and high resolution transmission electron microscopy. Rutile, anatase, and brookite precipitated on the interface between {110} planes of mullite and glass pockets in the sintered body. The formation of brookite may be attributable to the Si- and Al-rich environment during precipitation. Each polymorph of titania has a unique morphology and orientation relationship with mullite. Brookite exhibits a truncated pill box shape, and anatase displays a vermicular morphology. Quenching experiments suggest that the precipitates grow and undergo phase transformations during cooling.


NANO ◽  
2018 ◽  
Vol 13 (10) ◽  
pp. 1850119
Author(s):  
Xiaoyan Li ◽  
Yunlong Yu ◽  
Xiangfeng Guan ◽  
Peihui Luo ◽  
Linqin Jiang ◽  
...  

Eu[Formula: see text]/Tb[Formula: see text] co-doped nanocomposite containing CeO2 nanocrystals was successfully prepared by an in situ sol–gel polymerization approach. High-resolution transmission electron microscopy demonstrated the homogeneous precipitation of CeO2 nanocrystals among the polymethylmethacrylate (PMMA) matrix. The thermal stability and UV-shielding capability of the obtained nanocomposite were improved with increase of CeO2 content. The tuning of the emissive color from green and yellow to red can be easily achieved by varying the dopant species and concentration. These results suggested that the obtained nanocomposite could be potentially applicable in transparent solid-state luminescent devices.


2007 ◽  
Vol 124-126 ◽  
pp. 1165-1168 ◽  
Author(s):  
M. Qamar ◽  
Cho Rong Yoon ◽  
Hyo Jin Oh ◽  
Anna Czoska ◽  
K. Park ◽  
...  

The TiO2 sol was prepared hydrothermally in an autoclave from aqueous TiOCl2 solutions as starting precursor. Hollow fibers were obtained when sol-gel derived TiO2 sol was treated chemically with NaOH solution and subsequently heated in autoclave under various conditions. A systematic analysis of the influence of different NaOH concentrations on the formation of nanotubes has been carried out using XRD and SEM. The phase structure of the synthesized material was determined by transmission electron microscopy and found that these materials are, infact, hollow fibers widely known as nanotubes. From the TEM images, the outer and inner diameters of the tubes were measured ca. 8 and about 4 nm, respectively, with several hundred nanometers in length.


1999 ◽  
Vol 14 (12) ◽  
pp. 4570-4580 ◽  
Author(s):  
M. Alguerá ◽  
M. L. Calzada ◽  
L. Pardo ◽  
E. Snoeck

Transmission electron microscopy has shown that the grain size of sol-gel-prepared lanthanum-modified lead titanate films increases from ∼100 to ∼1 μm when the excess of PbO in the precursor solution is reduced from 20 to 10 mol%. Switchable polarization is higher in the films with a smaller grain size. Profilometry and the temperature dependence of the dielectric permittivity indicate that films are tensile stressed by the substrate. The grain-size effect on polarization switching is explainedby taking into account this tensile stress, which is thought to induce some a-domain orientation and 90° domain wall clamping in the grains attached to the substrate.


2014 ◽  
Vol 20 (4) ◽  
pp. 1271-1275 ◽  
Author(s):  
Wentao Qin ◽  
Donavan Alldredge ◽  
Douglas Heleotes ◽  
Alexander Elkind ◽  
N. David Theodore ◽  
...  

AbstractSilicon oxide used as an intermetal dielectric (IMD) incorporates oxide impurities during both its formation and subsequent processing to create vias in the IMD. Without a sufficient degassing of the IMD, oxide impurities released from the IMD during the physical vapor deposition (PVD) of the glue layer of the vias had led to an oxidation of the glue layer and eventual increase of the via resistances, which correlated with the O-to-Si atomic ratio of the IMD being ~10% excessive as verified by transmission electron microscopy (TEM) analysis. A vacuum bake of the IMD was subsequently implemented to enhance outgassing of the oxide impurities in the IMD before the glue layer deposition. The implementation successfully reduced the via resistances to an acceptable level.


1995 ◽  
Vol 10 (5) ◽  
pp. 1264-1269 ◽  
Author(s):  
G. Pacheco-Malagon ◽  
A. Garcia-Borquez ◽  
D. Coster ◽  
A. Sklyarov ◽  
S. Petit ◽  
...  

Nanosized TiO2 is synthesized in a nanosized alumina matrix by a sol-gel procedure. The results of the study of the blueshift of the TiO2 UV band edge are compared to the information obtained from transmission electron microscopy (TEM). As long as the atomic ratio Ti/Al remains smaller than 17.5%, no individualized TiO2 particles are detected by TEM, in spite of the fact that no modification of the alumina structure occurs, as revealed by 27Al MAS NMR. The shift of the UV band edge suggests the growth of homogeneous TiO2 domains in the alumina matrix. Above a critical radius, on the order of 1.2 nm, individual and crystalline TiO2 particles become visible in the TEM picture, and the porosity of the material decreases markedly.


2014 ◽  
Vol 886 ◽  
pp. 36-40
Author(s):  
Rong Hua Zhang ◽  
Bao Hong Zhu ◽  
Xiao Ping Zheng

Heat-resistant Al-8.5Fe-1.3V-1.7Si aluminum alloys were prepared by spray forming technique. The phase transition of deposited alloys from room temperature to 500°C was measured by Differential Scanning Calorimeter. The organization and the second phases of the alloys were observed and studied by transmission electron microscopy. The research results show that No endothermic peak appears in the deposited alloys during heating process, there is no phase transition occur in the alloy during the heating process from room temperature to 500°C. The deposited alloys mainly include α-Al and α-Al12(Fe,V)3Si phase. Under the transmission electron microscopy, there are also a small amount of slug, fan-shaped, needle-like, block, strip second phases, these phases are Al12Fe3Si, Al8Fe2Si, θ-Al13Fe4, Al9FeSi3, Al6Fe.


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