Micro Pattern of TiO 2 Thin Film Formation by Direct Synthesis From Aqueous Solution and Transcription of Resist Pattern
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TiO 2 + 6F- + 4H
(1)
(1)
and that, when boric acid is added, the fluoride ion is consumed by reaction (2) BO 33- + 4F + 6H+ -- BF4- + 3H 2 0
(2)
then the chemical equilibrium in reaction (1) is shifted from left to right in order to increase the amount of fluoride ion, resulting in the formation of titanium oxide. We prepared a glass plate on which surface micro pattern with minimum line width of 1 m had been printed by commercial organic photoresist material (AZ1500, Hekist Corp.). Ammo423 Mat. Res. Soc. Symp. Proc. Vol. 623 © 2000 Materials Research Society
(2)
2
(
()analyzed b
(c •
nium hexafluorotitanate : (NH4 )2TiF6 was dissolved in distilled water. The glass plate was soaked in the solution as the substrate. We added boric acid to the solution. After the soaking, the substrate was washed with distilled water and dried at room temperature. No heat treatment was conducted. We name this soaking operation as the first soak. Then the glass plate was soaked in acetone or ethanol for 30 to 60 min. with ultrasonic vibration, which we name as "thesecond soak. The surface of the glass plate was by a thin-film X-ray diffraction [TF-XRD] (RINT-2500, Rigaku Co., Tokyo, Japan). Gold film was coated on the surface of the substrate, and scanning electron microscopic images were observed with a scanning electron microscope [SEMI (ESEM2700, Nikon Co., Tokyo, Japan). RESULTS and DISCUSSION
Characteristic peaks for anatase TiO 2 were observed in TF-XRD patterns for the glass plate after the first soak (Fig. 1). The intensity of the 004 reflection was the strongest. The orientation of (001) plane is indicated. In Fig. 2, SEM micrograph of the surface of the glass plate is given. The glass plate was coated with dense and homogeneous TiO2 thin film with around 0.2 /m thickness. This film was as hard as 6H to 7H pencils and attached to the glass surface strongly. In Fig. 3, SEM micrograph of the glass plate after the second soak is given. The resist material was dissolved off with TiO_ film just on and the micro pattern of TiO_ thin film transcribing the resist pattern was obtained. Various I I I I 50 40 30 20(CuKa)/° FIG. 1 (a) TF-XRD patterns of the glass plate after the first soak. (b) TF-XRD patterns of the glass plate not soaked. (c) Powder XRD pattern of reagent TiO 2 (anatase). I
20
micro pattern of TiO thin film are shown in Fig. 4. The minimum line width of the pattern was
1 ym. In Fig. 5, 60S. tilted SEM view of TiO 2 thin film was given. It is confirmed that the boundaries are clearly outlined.
I(X)
FIG. 2 SEM micrograph of the surface of the glass plate after the first soak.
Hm
iI(X)
lir
FIG. 3 SEM micrograph of the surface of the glass plate after the second soak.
424
FIG. 4 Various micro pattern of TiO 2 thin film. The minimum line width of the pattern was 1 m.
425
FIG. 5 60' tilted SEM view of TiO 2 thin film.
CONCLUSION TiO thin film was formed on the glass plate with micro pattern printed by resist material by using DSAS. The resist material was dissolved off with TiOa film just on by s
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