INSTITUTE OF PHYSICS PUBLISHING JOURNAL OF PHYSICS D: APPLIED PHYSICS
J. Phys. D: Appl. Phys. 40 (2007) 192–197 doi:10.1088/0022-3727/40/1/014
Fabrication and characterization of
ultra-water-repellent alumina–silica
composite films
Takahiro Ishizaki
1
, Nagahiro Saito
2
, Yasushi Inoue
1
,
Makoto Bekke
3
and Osamu Takai
1
1
EcoTopia Science Institute, Nagoya University, Furo-cho, Chikusa, Nagoya 464-8603,
Japan
2
Department of Molecular Design and Engineering, Graduate School of Engineering,
Nagoya University, Furo-cho, Chikusa, Nagoya 464-8603, Japan
3
Department of Materials Engineering, Graduate School of Engineering, Nagoya University,
Furo-cho, Chikusa-ku, Nagoya 464-8603, Japan
E-mail: ishizaki@eco-t.esi.nagoya-u.ac.jp
Received 5 July 2006, in final form 7 November 2006
Published 15 December 2006
Online at stacks.iop.org/JPhysD/40/192
Abstract
Ultra-water-repellent (UWR) films were prepared by microwave
plasma-enhanced chemical vapour deposition using trimethylmethoxysilane
and aluminium (III) diisopropoxide ethylacetoacetate (ADE) as raw
materials. The film was mainly composed of silica and alumina and was
apparently transparent. The film thickness was approximately 500 nm. The
sample surface was treated with an organosilane in order to introduce
hydrophobic groups. The hydrophobic modification led to a water contact
angle of more than 150
◦
, whose value corresponds to the UWR surface. The
hardness of film with an optimized Al content was significantly improved
compared with that without Al. The maximum hardness was 1.71 GPa. In
consequence, we successfully prepared an UWR film in the silica–alumina
system.
1. Introduction
Ultra-water-repellent (UWR) film has a water contact angle
of more than 150
◦
. The water drops on such a surface roll
over and over. The characteristic is expected to be applied
in various engineering productions such as eyeglasses, lenses
and automobile windows [1]. The UWR property is governed
by the chemical composition and geometrical structure of
surface [2, 3]. A surface becomes more hydrophobic with
a lowering of surface energy. As the simplest example, the
surface covered with CH
3
- or CF
3
-groups has low surface
energy and water repellent property [4]. However, the surface
energy is insufficient to produce UWR films. A suitable
roughness or surface texture is required for the UWR films
[5–7]. Thus, methods to provide roughness to solid surfaces
have been developed [8–17]. Many fabrication methods had
been employed to fabricate the UWR surfaces [18–37].
In order to realize the above-mentioned applications, it
is necessary for the UWR film to have good mechanical
properties. We have successfully fabricated thin films with
ultra-water repellency and high transparency by controlling
pressures of organosilane and CO
2
gases in microwave
plasma-enhanced chemical vapour deposition (MPECVD)
[38]. However, in the previous study, water contact angles
of the films were lowered with an increase in the hardness, and
the ultra-water repellency was changed into water repellency.
This was due to the decrease in surface roughness. We aim
to fabricate an UWR thin film with high hardness and high
transparency. In order to achieve this aim, we examined a
composite material in the silica–alumina system. The alumina
component would harden the UWR film without losing the
ultra-water repellency and transparency [39–41].
In this research, we report on an UWR film with
high hardness and transparency through MPECVD using
trimethylmethoxysilane (TMMOS, (CH
3
)
3
Si(OCH
3
)) and
(ADE) (C
12
H
23
AlO
5
) as raw materials. The water repellency
and hardness of the films were discussed from the viewpoint
of surface nanotextures, sliding angles and alumina content.
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