Heat treatment of spun-on acid-catalyzed sol-gel silica films

1994 ◽  
Vol 9 (3) ◽  
pp. 723-730 ◽  
Author(s):  
T.M. Parrill
Keyword(s):  
Heat Treatment ◽  
Refractive Index ◽  
Spin Coating ◽  
Compressive Strain ◽  
Sol Gel ◽  
Silica Films ◽  
Si Substrates ◽  
Acid Catalyzed ◽  
Film Porosity

SiO2 films, formed by spin coating acid-catalyzed TEOS-based sol-gel on Si substrates, were annealed at 300–1000 °C and analyzed using ellipsometry, FTIR, and in situ stress measurements. Film porosity ranged from an average of 28% before annealing to 7% after annealing 3 h at 1000 °C. Below ≍800 °C, water and silanol removal caused a decrease in refractive index and increase in the in-plane tensile stress. Infrared spectra indicated compressive strain normal to the plane, however. Above ≍800 °C, further densification and structural relaxation occurred. Exposure to H2O also caused relaxation after annealing, as the most compressed Si–O–Si units reacted preferentially with moisture.

Crystallization and Electrical Properties of Bi4TiO12 Films Derived from Bismuth Acetate and Bismuth Nitrate Precursor Solutions

1997 ◽  
Vol 493 ◽  
Author(s):  
Chang Jung Kim ◽  
C. W. Chung ◽  
Kyu Sang Lee
Keyword(s):  
Heat Treatment ◽  
Spin Coating ◽  
Glacial Acetic Acid ◽  
Ferroelectric Properties ◽  
Sol Gel ◽  
Bismuth Nitrate ◽  
Si Substrates ◽  
Nitrate Precursor ◽  
Coating Method ◽  
Double Heat Treatment

ABSTRACTFerroelectric Bi4Ti3O12 thin films were prepared by the sol-gel method to examine the effect of precursors on the variation of ferroelectric properties. Two kinds of Bi4Ti3O12 sol-gel precursor solutions were synthesized by dissolving bismuth acetate and bismuth nitrate in glacial acetic acid and then adding titanium acetate. The films were deposited on Pt coated Si substrates by the spin-coating method and crystallized by double heat-treatment. The Ps, the Pr, and the Ec values of the film derived from the Bi-acetate were 34.8 μC/cm2, 16.2 μC/cm2, and 128 kV/cm, respectively. The Ps, the Pr, and the Ec of the films from the Bi-nitrate were 14.2 μC/cm2, 5.7 μC/cm2, and 105 kV/cm, respectively. The Bi4T3O12 films prepared from the Bi-acetate revealed better ferroelectricity and resistivity compared to those obtained from the Bi-nitrate.

IN SITU FORMATION OF COBALT NANOCLUSTERS IN SOL–GEL SILICA FILMS FOR SINGLE-WALLED CARBON NANOTUBE GROWTH

NANO ◽  
2009 ◽  
Vol 04 (02) ◽  
pp. 99-106 ◽  
Author(s):  
LI WEI ◽  
BO WANG ◽  
DAPENG LIU ◽  
LAIN-JONG LI ◽  
YANHUI YANG ◽  
...  
Keyword(s):  
Thin Films ◽  
Photoelectron Spectroscopy ◽  
Spin Coating ◽  
Sol Gel ◽  
Preparation Condition ◽  
Fine Tuning ◽  
Silica Films ◽  
In Situ Formation ◽  
Carbon Nanotube Growth

A facile method was developed for in situ formation of Co nanoclusters in sol–gel silica thin films spin-coated on Si wafers. The size and density of Co nanoclusters can be controlled by spin-coating speeds, annealing methods, reduction temperatures under H 2, and metal precursor concentrations in tetraethylorthosilicate solutions. The optimized preparation condition, spin-coating speed of 9000 rpm, annealing at 500°C in air followed by reduction at 800°C in H 2, resulted in silica films as thin as 60 nm and Co nanoclusters with a mean diameter of 1.5 nm. Morphological and chemical characteristics of thin films and nanoclusters were studied by atomic force microscopy and X-ray photoelectron spectroscopy, respectively. Subsequently, these Co nanoclusters were successfully used to grow SWCNTs by CO decomposition. Film containing Co monometallic clusters produced SWCNTs of 1.3 nm in diameter, whereas film having Co/Mo bimetallic clusters produced SWCNTs of 0.9 nm. This sol–gel approach allowed not only easy catalyst patterning on a thin film but also a fine-tuning of SWCNT properties, e.g., diameter.

Preferred Orientations for Sol-Gel Derived Plzt Thin Layers

1993 ◽  
Vol 310 ◽  
Author(s):  
Toshihiko Tani ◽  
Zhengkui Xu ◽  
David A. Payne
Keyword(s):  
Heat Treatment ◽  
Surface Energy ◽  
Sol Gel ◽  
Nucleation And Growth ◽  
Thin Layers ◽  
Energy Conditions ◽  
Chemical Characteristics ◽  
Interfacial Chemistry ◽  
Si Substrates

AbstractPLZT thin layers were deposited onto various substrates by sol-gel methods, and crystallized under different conditions and substrate treatments. Relationships are given for the chemical characteristics of the substrate's surface and the preferred orientations which develop on heat treatment. A preferred (111) orientation always developed for perovskite crystallized on Pt layers which contained Ti on the surface. This was attributed to the formation of Pt3Ti and the role of heteroepitaxial nucleation and growth sites. In addition, a preferred (100) orientation was also obtained on unannealed Pt/Ti/SiO2/Si substrates which were free of Ti on the surface. This was attributed to self-textured growth with flat faces striving for minimum surface energy conditions. The results are discussed in terms of the importance of interfacial chemistry on the control of texture for crystallization of PLZT thin layers on coated substrates.

Chemical Analyses of Sol/Gel Surfaces and Thin Films

1984 ◽  
Vol 32 ◽  
Author(s):  
Carlo G. Pantano ◽  
C. A. Houser ◽  
R. K. Brow
Keyword(s):  
Thin Films ◽  
Photoelectron Spectroscopy ◽  
Sol Gel ◽  
Silica Films ◽  
Alumina Films ◽  
Surface Analysis Techniques ◽  
Relative Water ◽  
Temperature Programmed

ABSTRACTThe application of surface analysis techniques to the characterization of sol/gel surfaces and thin films is described. Secondary-ion mass spectroscopy (SIMS), x-ray photoelectron spectroscopy (XPS) and sputter-induced photon spectroscopy (SIPS) are used to measure the composition of multicomponent silicate films, the relative water content of alumina films, the nitrogen content of ammonia treated silica films, and the depth profiles for films on black chrome. The determination of chemical structure using XPS and SIMS is also discussed. Finally, a brief introduction to temperature-programmed desorption (TPD) and its potential for studying surface chemical reactions, in situ, is presented.

Stress Development in Low Dielectric Constant Silica Films During Drying and Heating Process

1999 ◽  
Vol 594 ◽  
Author(s):  
Mengcheng Lu ◽  
C. Jeffrey Brinker
Keyword(s):  
Dielectric Constant ◽  
Tensile Stress ◽  
Sol Gel ◽  
Low Dielectric Constant ◽  
Heating Process ◽  
Residual Tensile Stress ◽  
Silica Films ◽  
Stress Development ◽  
Low Dielectric

AbstractLow dielectric constant silica films are made using a surfactant templated sol-gel process (K∼2.5) or an ambient temperature and pressure aerogel process (K∼1.5). This paper will present the in-situ measurement and analysis of stress development during the making of these films, from the onset of drying till the end of heating. The drying stress is measured by a cantilever beam technique; the thermal stress is measured by monitoring the wafer curvature using a laser deflection method. During the course of drying, the surfactant templated films experience a low drying stress due to the influence of the surfactant on surface tension and extent of siloxane condensation. The aerogel films first develop a biaxial tensile stress due to solidification and initial drying. At the final stage of drying where the drying stress vanishes, dilation of the film recreates the porosity of the wet gel state, reducing the residual stress to zero. For the surfactant templated films, very small residual tensile stress remains after the heat treatment is finished (∼30MPa). Aerogel film has almost no measurable stress developed in the calcination process. In situ spectroscopic ellipsometry analysis during drying and heating, and TGA/DTA are all used to help understand the stress development.

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.

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