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Preparation and Characterization of Al2O3 Thin

Films from Liquid Phase.


Yoshifumi Horita, Tadataka Yasuda, Seichi Rengakuji,
*Yuuko Nakamura
Department of System Engineering of Materials and Life
Science,Faculty of Engineering, Toyama Univ.,*Center
for Institute Analysis, Toyama Univ.,
3190 Gofuku, Toyama-city, Toyama, 930-8555 Japan

Introduction
Al2O3 thin films are known as a material having
excellent properties such as heat resistance, corrosion
resistance, and friction resistance, etc. Various methods
for preparing thin film, e.g. ion plating, sputtering, sol-gel
method, have been carried out. Preparation of thin film by
sol-gel method has attractive features, such as its
simplicity, and the fact the process doesn’t need
expensive equipment.
In this experiment, we prepared the Al2O3 precursor
solution using the advanced sol-gel process and made a
Al2O3 thin film. To make hard-coating films, trials of
doping Co or Fe to Al2O3 were performed.
Fig1X-ray diffraction patterns of powder annealed at
various temperatures
Experiment
The Al2O3 precursor solution was prepared as below:
First, aluminum butoxide was prepared by reacting AlCl3
with butanol in toluene solvent, then reacting it with water
dissolved in butanol so that hydrolysis and polymerization
reaction occurred. The Al2O3 precursor solution was
condensed and diluted to 1mol/l. To make a harder film,
Co or Fe, which was supplied by CoCl2 or FeCl3 dissolved
in butanol, was added to Al2O3 precursor solution. This
was dried under an IR lamp, and then the powdered
product was heat-treated at several temperatures. The
structures of powders were measured by XRD.
The thin film was coated by dipping on glass or quartz
substrate. After drying the film under IR lamp and then
heat-treatment, the transmittance of the thin films was
measured by UV-vis. Surface roughness and morphology
of films were measured by AFM and FE-SEM.

Results and Discussion


XRD patterns of Al2O3 after heat-treatment are shown
in Fig.1. At about 700 to 800oC, - Al2O3 structures


appeared. At about 1000 , a mixture of g - Al2O3 and -


  

Al2O3 structurntified. XRD result of 3-atom % Co doped Fig2 X-ray diffraction patterns of powder annealed at
to Al2O3 thin filmes can be ide is shown Fig.2. The XRD various temperatures (Co doped)
peak of - Al2O3 crystallized at 1000oC shifted to a lower


angle. This peak shift is thought to be the formation of


solid solution. Al2O3 and Co or Fe doped films obtained
from precursor solution are transparent. The presence of
dissolved Co or Fe ion in Al2O3 is detected by UV-vis
spectra. From surface morphology in Fig.3, the grains
grow to about 30nm in diameter at 1000oC. X-ray
intensity becomes greater at higher temperature. AFM
image also shows the same trend.
Preparation of Al2O3 thin film is very easy by this method.
Moreover, the doping process is a very simple step, that
of mixing the material to Al2O3 precursor solution.

Fig.3. SEM image of Al2O3 thin film.

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