Phase Transformations in Sol-Gel PZT Thin Films

2000 ◽  
Vol 623 ◽  
Author(s):  
D.P. Eakin ◽  
M.G. Norton ◽  
D.F. Bahr
Keyword(s):  
Thin Films ◽  
Heat Treatment ◽  
Room Temperature ◽  
Structural Changes ◽  
Sol Gel ◽  
Ex Situ ◽  
Ambient Conditions ◽  
Crystalline Films ◽  
In Situ Heating

AbstractThin films of PZT were deposited onto platinized and bare single crystal NaCl using spin coating and sol-gel precursors. These films were then analyzed using in situ heating in a transmission electron microscope. The results of in situ heating are compared with those of an ex situ heat treatment in a standard furnace, mimicking the heat treatment given to entire wafers of these materials for use in MEMS and ferroelectric applications. Films are shown to transform from amorphous to nanocrystalline over the course of days when held at room temperature. While chemical variations are found between films crystallized in ambient conditions and films crystallized in the vacuum conditions of the microscope, the resulting crystal structures appear to be insensitive to these differences. Significant changes in crystal structure are found at 500°C, primarily the change from largely amorphous to the beginnings of clearly crystalline films. Crystallization does occur over the course of weeks at room temperature in these films. Structural changes are more modest in these films when heated in the TEM then those observed on actual wafers. The presence of Pt significantly influences both the resulting structure and morphology in both in situ and ex situ heated films. Without Pt present, the films appear to form small, 10 nm grains consisting of both cubic and tetragonal phases, whereas in the case of the Pt larger, 100 nm grains of a tetragonal phase are formed.

IN-SITU Analysis Of The Microstructure of Thermally Treated Thin Copper Films

1993 ◽  
Vol 309 ◽  
Author(s):  
J. Nucci ◽  
H. Neves ◽  
Y. Shacham ◽  
E. Eisenbraun ◽  
B. Zheng ◽  
...  
Keyword(s):  
Thin Films ◽  
Heat Treatment ◽  
Room Temperature ◽  
Thermal Evolution ◽  
Electron Beam Evaporation ◽  
Copper Films ◽  
Tem Analysis ◽  
Heat Treated ◽  
Baseline Information

AbstractCopper thin films were deposited by sputtering, electron beam evaporation, and electroless plating onto nitride membranes for TEM analysis. The samples were heat treated in-situ from room temperature to 600 °C for structural and chemical analysis. The as-deposited and heat treated microstructures were investigated. Orientation changes with heat treatment and reactions among the sample layers were analyzed by electron diffraction. This work provides baseline information for a study of the thermal evolution of copper lines.

scholarly journals Phase Evolution from Volborthite, Cu3(V2O7)(OH)2·2H2O, upon Heat Treatment

Minerals ◽  
2021 ◽  
Vol 11 (12) ◽  
pp. 1312
Author(s):  
Rezeda M. Ismagilova ◽  
Elena S. Zhitova ◽  
Sergey V. Krivovichev ◽  
Anastasia V. Sergeeva ◽  
Anton A. Nuzhdaev ◽  
...  
Keyword(s):  
Crystal Structure ◽  
Room Temperature ◽  
Analytical Data ◽  
Phase Evolution ◽  
Ex Situ ◽  
Fast Cooling ◽  
In Situ Heating ◽  
Structure Complexity ◽  
Increasing Temperature

In the experiments on volborthite in situ and ex situ heating, analogues of all known natural anhydrous copper vanadates have been obtained: ziesite, pseudolyonsite, mcbirneyite, fingerite, stoiberite and blossite, with the exception of borisenkoite, which requires the presence of As in the V site. The evolution of Cu-V minerals during in situ heating is as follows: volborthite Cu3(V2O7)(OH)2·2H2O (30–230 °C) → X-ray amorphous phase (230–290 °C) → ziesite β-Cu2(V2O7) (290–430 °C) → ziesite + pseudolyonsite α-Cu3(VO4)2 + mcbirneyite β-Cu3(VO4)2 (430–510 °C) → mcbirneyite (510–750 °C). This trend of mineral evolution agrees with the thermal analytical data. These phases also dominate in all experiments with an ex situ annealing. However, the phase compositions of the samples annealed ex situ are more complex: fingerite Cu11(VO4)6O2 occurs in the samples annealed at ~250 and ~480 °C and quickly or slowly cooled to room temperature, and in the sample annealed at ~850 °C with fast cooling. At the same time, blossite and stoiberite have been found in the samples annealed at ~480–780 and ~780–850 °C, respectively, and slowly cooled to room temperature. There is a trend of decreasing crystal structure complexity in the raw phases obtained by the in situ heating with the increasing temperature: volborthite → ziesite → mcbirneyite (except of pseudolyonsite). Another tendency is that the longer the sample is cooled, the more complex the crystal structure that is formed, with the exception of blossite, most probably because blossite and ziesite are polymorphs with identical crystal structure complexities. The high complexity of fingerite and stoiberite, as well as their distinction by Cu:V ratio, may explain the uncertain conditions of their formation.

Observation of the structural changes of sol-gel formed Li2MnTi3O8 during electrochemical reaction by in-situ and ex-situ studies

2015 ◽  
Vol 152 ◽  
pp. 187-194 ◽  
Author(s):  
Wei Chen ◽  
Hanfeng Liang ◽  
Lianyi Shao ◽  
Jie Shu ◽  
Zhoucheng Wang
Keyword(s):  
Structural Changes ◽  
Electrochemical Reaction ◽  
Sol Gel ◽  
Ex Situ

scholarly journals Structure-Dependent CO2 Gas Sensitivity of La2O2CO3 Thin Films

2017 ◽  
Vol 2017 ◽  
pp. 1-6 ◽  
Author(s):  
Margus Kodu ◽  
Tea Avarmaa ◽  
Hugo Mändar ◽  
Rando Saar ◽  
Raivo Jaaniso
Keyword(s):  
Thin Films ◽  
Partial Pressure ◽  
Low Cost ◽  
Sol Gel ◽  
Working Environment ◽  
Ex Situ ◽  
Potential Candidate ◽  
Gas Sensitivity ◽  
Sensor Structure

Rare earth oxycarbonates are potential candidate materials for constructing simple and low-cost chemiresistive sensors for monitoring carbon dioxide (CO2) gas in the living and working environment for personal comfort and health reasons. Also, measurement of CO2 concentrations is needed in many industrial processes. Specifically, sol-gel made nanoparticles of Nd and La oxycarbonates have been studied previously as novel CO2 gas sensor materials. In this paper, pulsed laser deposition of La oxycarbonate (La2O2CO3) thin films was studied and structural properties of obtained thin films were characterized. Also, CO2 gas sensing ability of synthesized films was evaluated. The films deposited under CO2 partial pressure in various conditions were all Raman amorphous. In situ or ex situ annealing procedure at high CO2 partial pressure was needed for obtaining crystalline La2O2CO3 films, whereby hexagonal and monoclinic polymorphs were obtained in ex situ and in situ processes, respectively. Sensor structure, made using in situ process, was sensitive to CO2 gas and showed relatively fast response and recovery characteristics.

Thermal stability of self-assembled ordered three-phase Au–BaTiO3–ZnO nanocomposite thin films via in situ heating in TEM

Nanoscale ◽  
2020 ◽  
Vol 12 (46) ◽  
pp. 23673-23681
Author(s):  
Shikhar Misra ◽  
Di Zhang ◽  
Ping Lu ◽  
Haiyan Wang
Keyword(s):  
Thin Films ◽  
Thermal Stability ◽  
Ex Situ ◽  
Three Phase ◽  
Nanocomposite Thin Films ◽  
Vertically Aligned ◽  
In Situ Heating ◽  
Self Assembled ◽  
Thermal Stability Of

Thermal stability of an ordered three-phase Au–BaTiO3–ZnO vertically aligned nanostructure by both ex situ annealing under air and vacuum conditions, and in situ heating in TEM in vacuum has been demonstrated.

scholarly journals Electron Beam Effects on Oxide Thin Films—Structure and Electrical Property Correlations

2019 ◽  
Vol 25 (3) ◽  
pp. 592-600 ◽  
Author(s):  
Krishna Kanth Neelisetty ◽  
Xiaoke Mu ◽  
Sebastian Gutsch ◽  
Alexander Vahl ◽  
Alan Molinari ◽  
...  
Keyword(s):  
Thin Films ◽  
Electron Beam ◽  
Structural Changes ◽  
Ex Situ ◽  
Structure Property ◽  
Oxide Thin Films ◽  
Tem Characterization ◽  
Characterization Studies ◽  
Property Correlations

AbstractIn situ transmission electron microscope (TEM) characterization techniques provide valuable information on structure–property correlations to understand the behavior of materials at the nanoscale. However, understanding nanoscale structures and their interaction with the electron beam is pivotal for the reliable interpretation of in situ/ex situ TEM studies. Here, we report that oxides commonly used in nanoelectronic applications, such as transistor gate oxides or memristive devices, are prone to electron beam induced damage that causes small structural changes even under very low dose conditions, eventually changing their electrical properties as examined via in situ measurements. In this work, silicon, titanium, and niobium oxide thin films are used for in situ TEM electrical characterization studies. The electron beam induced reduction of the oxides turns these insulators into conductors. The conductivity change is reversible by exposure to air, supporting the idea of electron beam reduction of oxides as primary damage mechanism. Through these measurements we propose a limit for the critical dose to be considered for in situ scanning electron microscopy and TEM characterization studies.

X-ray Diffraction Investigations of TiO2 Thin Films and Their Thermal Stability

2011 ◽  
Vol 1352 ◽  
Author(s):  
Radomír Kužel ◽  
Lea Nichtová ◽  
Zdeněk Matěj ◽  
Zdeněk Hubička ◽  
Josef Buršík
Keyword(s):  
Thin Films ◽  
Room Temperature ◽  
Annealing Temperature ◽  
Sol Gel ◽  
Laboratory Measurements ◽  
X Ray Diffraction ◽  
Tio2 Thin Films ◽  
X Ray ◽  
Sol Gel Films

ABSTRACTIn-situ laboratory measurements in X-ray diffraction (XRD) high-temperature chamber and detailed XRD measurements at room temperature were used for the study of the thickness, temperature and time dependences of crystallization of amorphous TiO2 thin films. The films deposited by magnetron sputtering, plasma jet sputtering and sol-gel method were analyzed. Tensile stresses were detected in the first two cases. They are generated during the crystallization and inhibit further crystallization that also depends on the film thickness. XRD indicated quite rapid growth of larger crystallites unlike the sol-gel films when the crystallites grow mainly by increasing of annealing temperature.

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