Microstructural Evolution of Sol-Gel Derived PZT Thin Films

1991 ◽  
Vol 243 ◽  
Author(s):  
Cheng-Chen Hsueh ◽  
Martha L. Mecartney

AbstractTransmission electron microscopy (TEM) was used to investigate the microstructural evolution of sol-gel derived ferroelectric PZT films. Aggregates of perovskite crystals nucleated and grew out of a pyrochlore matrix at 550°C. A dense, single-phase perovskite PZT film was obtained by fast firing the film at 650°C for 30 minutes. The grain size of this film was approximately 0.2-0.4 μm. Hot-stage TEM observed disappearance of ferroelectric domains as the temperature approaching 325°C.

2012 ◽  
Vol 1427 ◽  
Author(s):  
Kanu priya Sharma ◽  
Thomas Oseroff ◽  
Leda Lunardi

ABSTRACTCrack free lead zirconate titanate (PZT) films for piezoelectric based MEMS devices have been prepared by a multiple coating sol gel process on platinized silicon (100) substrates. Rapid thermal annealing and Conventional furnace annealing were used for densification and crystallization of the amorphous PZT films. Scanning electron microscopy (SEM), Transmission electron microscopy (TEM) and Atomic force microscopy (AFM) were used to observe surface film morphology and grain growth. The phase content of the films was analyzed using X-ray diffraction. The role of intermetallics formed during the heat treatment in the growth of different orientations has also been observed. Film aging critical for device performance has been observed and methods to revert aging effects have been examined and discussed.


2021 ◽  
Author(s):  
V Maphiri ◽  
L Melato ◽  
Mhlongo ◽  
TT Hlatshwayo ◽  
TE Motaung ◽  
...  

Abstract Un-doped and ZnAlxO(1.5x + 1):0.1% Tb3+ (ZAOT) nano-powders were synthesized via citrate sol-gel method. The Alx moles were varied in the range of 0.25 ≤ x ≤ 5.0. The X-ray powder diffraction (XRD) data revealed that for the x < 1.5, the prepared samples crystal structure consists of mixed phases of the cubic ZnAl2O4 and hexagonal ZnO phases, while for the x ≥ 1.5 the structure consists of single phase of cubic ZnAl2O4. This was confirmed by the Raman and Fourier-Transform Infrared (FTIR) vibrational spectroscopy. Scanning electron microscopy (SEM) showed that varying Alx moles influences the morphology while Transmission electron microscopy (TEM) shows the dual morphology at x < 1.5. The photoluminescence (PL) revealed intense and distinct emissions attributed to both the host and Tb3+ transitions. The emission intensity highly depends on the Alx moles. The International Commission on Illumination (CIE) colour chromaticity showed that the emission colour could be tuned by varying the Alx moles.


1998 ◽  
Vol 541 ◽  
Author(s):  
S.P. Alpay ◽  
V. Nagarajan ◽  
L.A. Bendersky ◽  
M.D. Vaudin ◽  
S. Aggarwal ◽  
...  

AbstractThe domain structure of the 400 nm thick PbZr0.2Ti0.8O3 (PZT) films with different electrode layer configurations was investigated by x-ray diffraction and transmission electron microscopy. The c-domain fractions of the PZT films with no electrode layer, with a 50 nm electrode layer between the film and the substrate, and with 50 nm electrode layers on top and bottom of the PZT film were found to be equal. This means that depolarizing fields do not affect the polydomain structure of the film. Calculations of the in-plane strains based on the lattice parameters of the La0.5Sr0.5CoO3 (LSCO) layer in the above configurations led to the conclusion that the bottom electrode layer is coherently strained to match the substrate.


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.


2007 ◽  
Vol 280-283 ◽  
pp. 239-242 ◽  
Author(s):  
Wen Gong ◽  
Xiang Cheng Chu ◽  
Jing Feng Li ◽  
Zhi Lun Gui ◽  
Long Tu Li

Lead zirconate titanate (PZT) thin films with a composition near the morphotropic phase boundary were deposited on silicon wafers by using a modified sol-gel method. Introducing a seeding layer between the interface of PZT film and platinum electrode controlled the texture of PZT films. The lead oxide seeding layer results in highly (001)-textured PZT film, while the titanium dioxide seeding layer results in (111)-textured one. SEM and XRD were used to characterize the PZT thin films. The ferroelectric and piezoelectric properties of the PZT films were evaluated and discussed in association with different preferential orientations.


1992 ◽  
Vol 271 ◽  
Author(s):  
G. Teowee ◽  
J. M. Boulton ◽  
D. R. Uhlmann

ABSTRACTA series of PZT precursor solutions was prepared which incorporated excess PbO to give the composition Pb1+xZr0.53Ti0.47O3+x, where 0 < × < 0.3. These solutions were spin coated on platinized Si wafers and fired at elevated temperatures up to 750C for 30 mins. After crystallization into single-phase perovskite, the films were studied using XRD, optical microscopy and electrical characterization techniques (hysteresis loops and dielectric properties). It was found that the presence of excess PbO significantly improved the PZT films in terms of phase assemblage, microstructure and electrical properties. Under optimized conditions, films with dielectric constants of around 3000 can be obtained.


1993 ◽  
Vol 310 ◽  
Author(s):  
Supapan Seraphin ◽  
Dan Zhou ◽  
G. Teowee ◽  
J.M. Boulton ◽  
D.R. Uhlmann

AbstractThe microstructure of lead zirconate titanate (PZT) thin films prepared by a sol-gel technique was investigated using transmission electron microscopy (TEM) and transmission electron diffraction. We investigated the microstructure of three sets of thin films with different chemical compositions: PZT 53/47 films with no excess PbO; with excess PbO; and PZT 65/35 with no excess PbO. All samples were fired for 30 minutes at temperatures ranging from 400C to 700C. Incorporation of excess PbO in the 53/47 film fired at 450C resulted in polycrystalline perovskite grains with an average grain size of less than 0.1 μm. Grain boundaries are decorated by 5-10 nm diameter precipitates possibly caused by the segregation of remnant pyrochlore or excess PbO. The films have high values of dielectric constant (up to 2500) when fired at 700C. PZT 65/35 fired at 700C consists of two distinct phases: a fine-grained matrix of pyrochlore, and 10-μm diameter rosettes of perovskite. The correlations between the compositions, the microstructure of the films, and their processing conditions on the one hand, and ferroelectric properties on the other are discussed.


2005 ◽  
Vol 475-479 ◽  
pp. 1583-1586
Author(s):  
Wen Gong ◽  
Jing Feng Li ◽  
Xiang Cheng Chu ◽  
Long Tu Li

Pb(Zr,Ti)O3 (PZT) thin films have attracted great attention due to their superior ferroelectric, pyroelectric and piezoelectric properties. The epitaxial films on single-crystal substrates are expected to possess enhanced properties compared with polycrystalline films on conventional silicon wafers. We prepared epitaxial PZT films on STO (STO) substrates with different orientation by using a sol-gel method. The preparation parameters were optimized to improve crystallization of the films. Although the films were of the same composition and prepared under the same condition, different crystal phases with corresponding preferential film orientations were formed when the substrate orientation was changed. [001]-oriented tetragonal PZT film was formed on the {100} surface of the STO substrate, whereas [111]-oriented rhombohedral PZT film on the {111} surface.


2011 ◽  
Vol 65 (5) ◽  
Author(s):  
Helena Bruncková ◽  
Ľubomír Medvecký ◽  
Pavol Hvizdoš

AbstractDouble-scale composite lead zirconate titanate Pb(Zr0.52Ti0.48)O3 (PZT) thin films of 360 nm thickness were prepared by a modified composite sol-gel method. PZT films were deposited from both the pure sol and the composite suspension on Pt/Al2O3 substrates by the spin-coating method and were sintered at 650°C. The composite suspension formed after ultrasonic mixing of the PZT nanopowder and PZT sol at the powder/sol mass concentration 0.5 g mL−1. PZT nanopowder (≈ 40–70 nm) was prepared using the conventional sol-gel method and calcination at 500°C. Pure PZT sol was prepared by a modified sol-gel method using a propan-1-ol/propane-1,2-diol mixture as a stabilizing solution. X-ray diffraction (XRD) analysis indicated that the thin films possess a single perovskite phase after their sintering at 650°C. The results of scanning electron microscope (SEM), energy-dispersive X-ray (EDX), atomic force microscopy (AFM), and transmission electron microscopy (TEM) analyses confirmed that the roughness of double-scale composite PZT films (≈ 17 nm) was significantly lower than that of PZT films prepared from pure sol (≈ 40 nm). The composite film consisted of nanosized PZT powder uniformly dispersed in the PZT matrix. In the surface micrograph of the film derived from sol, large round perovskite particles (≈ 100 nm) composed of small spherical individual nanoparticles (≈ 60 nm) were observed. The composite PZT film had a higher crystallinity degree and smoother surface morphology with necklace clusters of nanopowder particles in the sol-gel matrix compared to the pure PZT film. Microstructure of the composite PZT film can be characterized by a bimodal particle size distribution containing spherical perovskite particles from added PZT nanopowder and round perovskite particles from the sol-matrix, (≈ 30–50 nm and ≈ 100–120 nm), respectively. Effect of the PZT film preparation method on the morphology of pure and composite PZT thin films deposited on Pt/Al2O3 substrates was evaluated.


2007 ◽  
Vol 22 (6) ◽  
pp. 1737-1743 ◽  
Author(s):  
A. Pohl ◽  
G. Westin

An all-alkoxide sol-gel route to the formation of Nd1/3La1/3Ca1/3MnO3thin films and powders has been developed. The microstructural evolution on heat treatment of the gel to yield the perovskite oxide was monitored by means of thermogravimetric analysis-differential scanning calorimetry, powder x-ray diffraction (XRD), Fourier transform infrared spectroscopy, and transmission electron microscopy (TEM)-energy dispersive spectroscopy (EDS). It was found that the amorphous gel consists of hydrated oxo-carbonate without organic residues, and on heating it decomposes in several steps, finally forming single-phase perovskite at 680 °C. Further heating results in only slight changes in the cell parameters and crystal growth. Films were prepared by spin coating, followed by heat treatment in air to a temperature of 800 °C, and studied by scanning electron microscopy, TEM-EDS, and XRD. Films on Al2O3were more porous, while films on Pt–TiO2–SiO2–Si were rather dense and consisted of areas with different crystal orientations.


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