ELSEVIER Thin SolidFilms 304 (1997) 222-224
Chemical vapor deposition of A1203 films using highly volatile single
sources
Wonyong Koh, Su-Jin Ku, Yunsoo Kim
Thin Film Materials Laborator); Korea Research Institute of Chemical Technology, Yusong P.O. Box 107, Taejon 305-600, South Korea
Received2 January 1997; accepted26 February 1997
Abstract
Amorphous AI203 films were grown on Si(100) and Si(11 l) substrates by low-pressure chemical vapor deposition in the temperature
range of 250-600°C using dimethylaluminum isopropoxide, dimethylaluminum tert-butoxide, and diethylaluminum isopropoxide as
single sources. All these sources vaporize readily at room temperature under reduced pressure. The films were characterized by X-ray
diffractometry, X-ray photoelectron spectroscopy, Auger electron spectroscopy and scanning electron microscopy. Auger depth profiling
analysis of the samples indicates no appreciable carbon incorporation in the films. © 1997 Elsevier Science S.A.
Keywords: Aluminumoxide; Chemical vapor deposition; Depth profiling; Organometallicvapor deposition
Films and coatings of aluminum oxide (A120 3) have
numerous electrical, optical and wear-resistant applica-
tions. A120 3 films are commonly produced by chemical
vapor deposition (CVD) using various kinds of aluminum
sources such as aluminum chloride, aluminum isopropox-
ide (A1(O-iC3I-I7)3), aluminum tert-butoxide (AI(O-
tC4H9)3), aluminum acetylacetonate, aluminum hexafluo-
roacetylacetonate, trimethylaluminum (AI(CH3)3), and
aluminum 2-ethylhexanoate, and these are well reviewed
recently [1]. Aluminum borohydride (AI(BH4)3) [21 and
aluminum 2,2,6,6-tetramethyt-3,5-heptanedionate [3] are
also proposed as aluminum CVD sources. Among these
sources, only AI(CH3) 3 and AI(BH4) 3 are highly volatile
liquids whereas all the other sources are solids and must be
heated to temperatures higher than 100°C for vapor trans-
port. AI(CH3) 3 is commercially available and frequently
adapted for CVD of AI~O 3 [4-11]. However, it is py-
rophoric and must be handled carefully.
Using a single CVD source provides a novel alternative
to conventional CVD that employs separate sources for
each element of compound materials [12,13]. Gas-phase
mixing is not necessary and undesirable gas-phase reac-
tions that can generate particles or impurity sources are
* Corresponding author. E-mail: yunsukim@pado.krict.re.kr.
0040-6090/97/$17.00 © 1997 ElsevierScience S.A. All rights reserved.
PI1 S0040-6090(97)00132-6
much less likely to occur. Deposition usually proceeds at
lower temperatures compared to conventional CVD.
In this paper, we report on the CVD of Al20 3 films
using dimethylaluminum isopropoxide, (CH3)2AI(O-
iC3H7) , dimethylaluminum tert-butoxide, (CH3)2AI(O-
tC 4H 9 ), and diethylaluminum isopropoxide,
(C2I-Is)2AI(O-iC3Hv), as single sources. These com-
pounds can be synthesized at room temperature simply by
mixing AI(CH3) 3 or AI(CzHs) 3 with AI(O-iC3HT) 3 or
AI(O-tC4Hg) 3 in a 2:1 ratio under inert atmosphere.
(CH3)2AI(O-iC3H 7) is a liquid whereas (CH3)2AI(O-
tC4H 9) and (C2Hs)zAI(O-iC3H 7) are gel-like solids.
Si(100) and Si(lt 1) substrates were degreased and cleaned
just prior to CVD. A simple CVD apparatus was used in
which borosilicate glass tubing, quartz tubing, and stain-
less steel bodies are connected through O-ring joints. It
was evacuated by a rotary vane pump only. No carrier gas
was used and the sources vaporized at room temperature.
The substrates were placed on a graphite heating block.
Substrate temperature was monitored by a thermocouple
inserted in the graphite block. The deposition temperature
was maintained in the range of 250-600°C. The pressure,
measured by a Convectron gauge, was initially about 1 Pa
and increased to 4-10 Pa after introducing a source into
the apparatus. Interference colors of transparent oxide
films on the substrates were observed within several min-
utes after starting the CVD, which continued for several
hours.