Metalorganic chemical vapor deposition of oxide films on semiconductor substrates using aluminum, gallium, and indium alkyl chloride precursors

Article abstract of DOI:10.1023/A:1015454518259

The thermal decomposition of dipropylaluminum, dipropylgallium, and dipropylindium chlorides was investigated by thermal analysis. The growth kinetics of oxide films on silicon and gallium arsenide were studied, using dipropylaluminum, dipropylgallium, an

Full text of DOI:10.1023/A:1015454518259

Inorganic Materials, Vol. 38, No. 5, 2002, pp. 438–444. Translated from Neorganicheskie Materialy, Vol. 38, No. 5, 2002, pp. 539–545.
Original Russian Text Copyright © 2002 by Mittov, Ponomareva, Mittova.
Metalorganic Chemical Vapor Deposition of Oxide Films
on Semiconductor Substrates Using Aluminum, Gallium,
and Indium Alkyl Chloride Precursors
†
O. N. Mittov , N. I. Ponomareva, and I. Ya. Mittova
Voronezh State University, Universitetskaya pl. 1, Voronezh, 394693 Russia
e-mail: xelga@mailru.com
Received July 9, 2001; in final form, October 19, 2001
Abstract—The thermal decomposition of dipropylaluminum, dipropylgallium, and dipropylindium chlorides
was investigated by thermal analysis. The growth kinetics of oxide films on silicon and gallium arsenide were stud-
ied, using dipropylaluminum, dipropylgallium, and dipropylindium chlorides; propylaluminum and propylgal-
lium dichlorides; ethylaluminum dichloride; and diethylaluminum and diethylindium chlorides as metalorganic
precursors. The resultant films were characterized by IR and x-ray spectroscopies and electrical measurements.
INTRODUCTION
found to depend strongly on the process parameters.
Oxide films were also produced using alkoxide precur-
sors, in particular aluminum isopropoxide [13–17].
Chemical vapor deposition (CVD) of oxide films
using metalorganic (MO) or organosilicon precursors is
widely employed to produce insulator layers of capaci-
tors and metal–insulator–semiconductor (MIS) struc-
tures, protective and sealing layers, and masking films
for semiconductor doping [1]. MOCVD plays a key role
in the fabrication of semiconductor devices on III–V
substrates because these may decompose at relatively
low temperatures. The low structural perfection of the
native oxide layer on gallium arsenide stimulates the
search for low-temperature methods of growing oxide
films on this material. In this context, there is consider-
able interest in Group IIIA MO compounds. As shown
earlier [2], oxidation of gallium arsenide under mild
conditions yields an oxide layer consisting predomi-
nantly of Ga2O3. Therefore, thermal decomposition of
MO precursors is expected to offer relatively high dep-
osition rates of Ga2O3, Al2O3, or In2O3, which are
known to be similar in physicochemical properties.
Moreover, this process may ensure enhanced adhesion
and healing of structural defects.
Al2O3 and In2O3 films were also grown by alkyl
technology [18, 19]. The use of this technique is how-
ever limited by the high reactivity of metal alkyl com-
pounds with air and moisture. To reduce the extremely
high reactivity of trimethylgallium etherate, Armer and
Schmidbauer [20] dissolved it in diethyl ether and
could obtain Ga2O3 layers on gallium arsenide at lower
temperatures than in the case of the acetylacetonate
precursor. It is of interest to examine the possibility of
using MO precursors more stable than metal alkyl com-
pounds, e.g., aluminum, gallium, and indium alkyl
halides. Such precursors have been used in only a few
studies. For example, Piloyan and Novikova [21]
reported the preparation of gallium arsenide epilayers
using diethylgallium chloride.
The objective of this work was to grow oxide films
on Si and GaAs by MOCVD using dipropylaluminum
chloride (DPAC), dipropylgallium chloride (DPGC),
dipropylindium chloride (DPIC), propylaluminum
dichloride (PADC), propylgallium dichloride (PGDC),
ethylaluminum dichloride (EADC), diethylaluminum
chloride (DEAC), and diethylindium chloride (DEIC)
as precursors and to investigate the composition and
properties of the films.
Among suitable precursors for MOCVD of oxide
films are alkyls, acetylacetonates, alkoxides, carboxy-
lates, and phenolates [1]. If an MO precursor contains lit-
tle or no oxygen, the process must be run in an oxidizing
atmosphere (oxygen, water vapor, or carbon dioxide).
The most common precursors are metal acetylacetonates.
The preparation of Al2O3 and In2O3 via thermal decom-
position of aluminum and gallium acetylacetonates was
described in many reports [3–12]. The oxide films were
deposited on glass, quartz, nickel, tantalum, silicon, and
germanium but not on III–V semiconductors. The com-
position, structure, and properties of the deposits were
EXPERIMENTAL
The MO precursors were synthesized by reacting
tripropylaluminum, tripropylgallium, and tripropylin-
dium with hydrogen chloride [21].
As substrates, we used polished wafers of AGChT
GaAs(100) with a carrier concentration of 1016 cm–3
and KEF Si with an electrical resistivity of 0.3 Ω cm.
†
Deceased.
0020-1685/02/3805-0438$27.00 © 2002 MAIK “Nauka/Interperiodica”

METALORGANIC CHEMICAL VAPOR DEPOSITION OF OXIDE FILMS
439
t, °C
400
350
300
250
200
150
t, °C
T
T
400
DTG
DTG
−∆m, mg
–∆m, mg
300
0
DTA
10
DTA
20
30
40
20
40
60
80
200
50
60
70
TG
100
50
80
100
50
90
100
TG
5
10 15 20 25 30 35
15
20
25
30 35 40
Time, min
Time, min
Fig. 1. Thermal analysis of DPAC.
Fig. 2. Thermal analysis of DPGC.
The process was run in a resistance-heated two-zone
furnace. The temperature was maintained with a stabil-
ity of ±1°C. The source and deposition temperatures
were chosen using thermoanalytical (DTA + TG +
DTG) data (Paulik–Paulik–Erdey system).
DPAC decomposes in one step between 50 and
390°C, with a maximum in decomposition rate at
350°C (Fig. 1). The total weight loss amounts to
70.66%. The heating curve shows two endotherms
(190–240 and 340–350°C) and one exotherm (325–
We used single- and two-zone procedures. In the
former case, the MO precursor was placed in a quartz
container, which was then covered with the substrate.
In the two-zone procedure, the container with the pre-
cursor was situated in the lower temperature zone,
where the precursor vaporized without decomposition,
and the substrate was located in the higher temperature
zone, where the precursor decomposed. The single-
zone procedure ensured higher deposition rates, and the
two-zone procedure provided layers more uniform in
thickness. Deposition was carried out in air or a mixture
of oxygen and argon carrier gas. The flow rate of argon
was 15 l/h, and that of oxygen was 13 l/h.
Film thicknesses were measured with an E-3 ellip-
someter to an accuracy of ±1 nm. Film composition
was determined by IR spectroscopy (UR-20 instru-
ment) and ultrasoft x-ray emission spectroscopy (RSM-
500 instrument). In current–voltage (I–V) and capaci-
tance–voltage (C–V) measurements, we used MIS
structures.
t, °C
DTG
0
T
−∆m, mg
0
500
400
300
DTA
10
20
30
40
200
100
TG
RESULTS AND DISCUSSION
5
10
20 30 40
Time, min
50
The source and substrate temperatures were chosen
based on thermoanalytical data, as illustrated in
Figs. 1–3 for DPAC, DPGC, and DPIC.
Fig. 3. Thermal analysis of DPIC.
INORGANIC MATERIALS Vol. 38 No. 5 2002

440
MITTOV et al.
involves an endothermic event at 105–115°C and an
1000
800
600
400
200
2
exothermic event at 130–170°C. The second step
involves a weight loss of 12.86% and an exothermic
event in the range 300–370°C.
DPIC also decomposes in two steps (Fig. 3). The
first step occurs in the range 80–300°C, with a maxi-
mum in decomposition rate at 140°C, and involves a
weight loss of 31.48% and an endothermic event at
60−125°C. The second step (300–500°C, maximum
decomposition rate at 440°C) is accompanied by a
weight loss of 50% and involves exothermic and endot-
hermic events between 325 and 400°C.
1
0
1
2
3
4
5
6
7
8
9
Time, min
The exotherms indicate that the decomposition of
the MO precursors is accompanied by oxidation of the
metal with atmospheric oxygen.
Fig. 4. Film thickness as a function of deposition time for
DPGC pyrolysis in air at (1) 125 and (2) 150°C; GaAs sub-
strate.
Table 1 lists the activation energies Ea for the
decomposition of DPAC, DPGC, and DPIC, calculated
as described in [22] and by the method of successive
approximations reported in [23], which makes it possi-
ble to assess kinetic parameters using a limited number
of data points. Analysis of the data in Figs. 1–3 and
Table 1 indicates that the activation energies calculated
by the two methods coincide only if there is a sufficient
number of data points in the same temperature range.
The rather low values of Ea demonstrate that the com-
pounds in question decompose readily in the range
350–500°C and can be used as MO precursors for the
deposition of oxide films by MOCVD in an oxidizing
atmosphere.
330°C). DPGC decomposes in two steps (Fig. 2). The
first step (20–250°C, maximum decomposition rate at
140°C) is accompanied by a weight loss of 41.42% and
Table 1. Activation energies for the decomposition
of DPAC, DPGC, and DPIC extracted from thermoanalytical
data
MO precursor
(C3H7)2AlCl
t, °C
Ea, kJ/mol
100–170
180–270
280–315
335
9 ± 4
9 ± 1
35 ± 7
106 ± 20*
28 ± 5
14 ± 2*
7 ± 1
The above results enabled us for the first time to pro-
duce oxide films via DPAC, DPGC, and DPIC pyroly-
sis. The temperature ranges of the MOCVD process
were assessed from thermoanalytical results. The
experiments were however complicated by the instabil-
ity of the MO precursors in air. Oxide films on GaAs
could be prepared by decomposing DPGC in air by the
single-zone procedure in the range 125–300°C. How-
ever, the results were poorly reproducible, because
DPGC is unstable in air, especially at elevated temper-
atures, and the growth kinetics of the films were diffi-
cult to follow. Systematic measurements were made
only at 125 and 150°C (Fig. 4). The film thickness was
found to increase linearly with deposition time, charac-
teristic of pyrolytic decomposition processes. The rate
constants for film deposition via DPGC pyrolysis are
listed in Table 2, together with the parameters of a lin-
ear rate equation for two-zone DPGC pyrolysis in an
oxygen–argon mixture. The film thickness vs. deposi-
tion time data for this process are displayed in Fig. 5.
(C3H7)2GaCl
100–120
100
120–140
140–400
390
6 ± 1
25 ± 7*
33 ± 3
7 ± 1
(C3H7)2InCl
60–110
120–170
200–320
350–410
390
6 ± 1
34 ± 3
37 ± 2*
* Calculated by the method of successive approximations [23].
Table 2. Rate constants for film deposition via DPGC py-
rolysis
We failed to prepare quality films via DPAC pyroly-
sis in air between 200 and 350°C because this com-
pound is unstable at high temperatures. At 400°C in dry
oxygen, we obtained 430-nm-thick films by the single-
zone procedure in 1 min. At higher temperatures in
oxygen atmosphere, DPAC decomposes with an explo-
Procedure (atmosphere)
t, °C
K, nm/min
Single-zone (air)
125
150
300
40 ± 1
22 ± 1
18 ± 0.8
″
Two-zone (Ar + O2)
INORGANIC MATERIALS Vol. 38 No. 5 2002

METALORGANIC CHEMICAL VAPOR DEPOSITION OF OXIDE FILMS
441
sion. Diluting DPAC with toluene (1 : 1 by volume)
250
200
150
100
50
ensured a slower decomposition rate, and we were able
to produce films rather uniform in thickness. In this
way, we obtained a 425-nm-thick film at 400°C in
5 min.
2
1
With the aim of depositing In2O3 films, we exam-
ined DPIC pyrolysis at temperatures in the range
190−460°C. Although, according to thermoanalytical
data, DPIC decomposes at 400°C, we failed to obtain
oxide films between 190 and 400°C. The minimum
deposition temperature in air was 460°C. The thickness
of the films deposited at this temperature by the single-
zone procedure over a period of 5 min was 345 nm.
0
2
4
6
8
10
12
Time, min
Fig. 5. Film thickness as a function of deposition time for
the pyrolysis of (1) PADC at 400°C and (2) DPGC at 300°C
in a mixture of argon (15 l/h) and oxygen (13 l/h); GaAs
substrate.
The conditions for film deposition on GaAs sub-
strates via pyrolysis of the other MO precursors studied
are summarized in Table 3. In two runs (asterisked in
Table 3), the substrate was mounted on a holder situated
just ahead of the source. This prevented etching of the
growing film and made it possible to obtain uniform
thickness. The film thickness vs. deposition time data
for PADC pyrolysis are displayed in Fig. 5. The devia-
tion of the data from linearity is attributable to the fact
that, in the two-zone geometry, PADC partially decom-
poses (via pyrolysis and pyrohydrolysis) upstream of
the substrate, which reduces the deposition rate. The
growth kinetics can be represented by a power-law
which suggests that the deposition rate is limited by the
decomposition of the MO precursor just above the sub-
strate surface.
The Ga : As atomic ratios determined by ultrasoft
x-ray spectroscopy in the films produced using DPAC
and DPGC are given in Table 4. The energy scale was
calibrated against the µ2,3 lines of pure arsenic and gal-
lium. The Al content of the deposits could not be deter-
mined by this method. The measurements were made
on 0.7-µm-thick films under conditions which pre-
dependence d = Kτn, where n = 0.9 for the last process, vented penetration of x-rays into the substrate. All of
Table 3. Optimal conditions for film deposition on GaAs substrates via pyrolysis of aluminum, gallium, and indium alkyl
chloride precursors
MO precursor
t, °C
Oxidant
l, cm
τ, min
d, nm
C3H7AlCl2
350
440
470
460
460
460
470
470
360
460
460
460
Dry O2
1.0
1.0
1.0
0.6
0.6
1.2
1.2
1.2
0.6*
0.6
1.2
1.0*
5
50
125
226
100
1000
400
80
″
″
3
″
Air
2
C3H7GaCl2
″
2
″
″
5
″
″
2
C2H5AlCl2
″
1
″
″
1.5
3
1000
200
110
75
(C2H5)2AlCl
Dry O2
(C2H5)2InCl
Air
″
5
″
″
5
″
5
43
Note: l is the source–substrate distance, and d is film thickness.
* The substrate was situated on a holder just ahead of the source (see text).
INORGANIC MATERIALS Vol. 38 No. 5 2002

442
MITTOV et al.
Table 4. Ga : As atomic ratios in the films deposited on
GaAs using DPAC and DPGC (ultrasoft x-ray spectroscopy
data, deposition time of 3 min)
DPAC contained absorption bands at 1430 and
1590 cm–1, due to the Al–O bond [24]. The spectra of
the films deposited on Si using DPIC showed absorp-
tions at 900, 1430, and 1520 cm–1, corresponding to the
In–O bond. It is of interest that we also observed
absorptions at 470 and 525 cm–1, due to the Ga–O bond
[20], in the spectra of the films grown on Si and GaAs
using DPGC and the films grown on GaAs using DPAC
and DPIC.
MO precursor
t, °C
Ga : As
(C3H7)2AlCl
(C3H7)2GaCl
(C3H7)2GaCl
250
190
250
4 : 6
7 : 3
5 : 5
C–V and I–V measurements on MIS structures
showed that the substrate material had an insignificant
effect on the properties of the films (Table 5). The elec-
tric strength of the films was somewhat higher than that
of thermal oxide on gallium arsenide [2]. The large
fixed charge in the films can be explained by the rela-
tively low deposition temperature (≤300°C). Annealing
in argon at 400°C for 30 min reduced the charge in the
oxide films but increased film porosity, which could
then be reduced by additional annealing in water vapor
or humid oxygen.
the films were found to contain arsenic, even though the
deposition temperature was not high enough for GaAs
dissociation [2]. Gallium was present in the films
grown with the use of both Ga-containing precursors
and DPAC, indicating Ga diffusion from the substrate
to the film.
IR spectroscopic studies showed that the films
deposited on Si consisted of oxides of the correspond-
ing metal. The spectra of the films grown on Si using
Table 5. Electrical properties of the films deposited on GaAs and Si using DPAC, DPGC, and DPIC
MO precursor, substrate
t, °C
τ, min
Ebr × 10–5, V/cm
ε
ρ, Ω cm
(C3H7)2GaCl,
Si (KEF)
300
15
2.9
2.76
1.16 × 108
(C3H7)2GaCl,
GaAs
300
15
7.1
2.99
2.1 × 108
(AGChT-1)
(C3H7)2GaCl,
Si (KEF)
300
300
17
10
5.5
3.3
2.50
2.79
1.56 × 107
2.2 × 107
(C3H7)2GaCl,
GaAs
(AGChT-1)
(C3H7)2AlCl,
GaAs
400
460
1
5
9
3
–
–
–
–
(AGChT-1)
(C3H7)2InCl,
GaAs
(AGChT-1)
Note: E is the electric strength.
br
INORGANIC MATERIALS Vol. 38 No. 5 2002

METALORGANIC CHEMICAL VAPOR DEPOSITION OF OXIDE FILMS
443
primeneniyu MOS dlya polucheniya neorganicheskikh
pokrytii i materialov (Proc. V All-Union Conf. on the
Application of Metalorganic Precursors in the Prepara-
tion of Inorganic Coatings and Materials), Moscow:
Nauka, 1987, pp. 186–187.
CONCLUSION
Our results demonstrate that MOCVD with DPAC,
DPGC, and DPIC as precursors can be used to grow
insulator layers on gallium arsenide and silicon at tem-
peratures as low as 130–300°C. Of the dipropyl chlo-
ride precursors studied, DPIC is the least suitable for
the growth of oxide films: with this precursor, films
could not be produced by the two-zone procedure, and
the deposition temperature was rather high, presumably
because of its low volatility.
8. Korzo, V.F., Deposition of Thin Alumina Films by Ther-
mally Activated Decomposition of Organic Precursors,
Zh. Prikl. Khim. (Leningrad), 1976, vol. 49, no. 1,
pp. 74–77.
9. Korzo, V.F., Optical and Electrical Properties of Non-
crystalline Films, Izv. Akad. Nauk SSSR, Neorg. Mater.,
1976, vol. 12, no. 7, pp. 1224–1229.
The composition and properties of the oxide films
depend not only on the MO precursor but also on the
substrate material. Decomposition of the dipropyl chlo-
rides in an oxidizing atmosphere leads to both the dep-
osition of the corresponding metal oxide and the oxida-
tion of the GaAs substrate. The films produced via
DPAC pyrolysis at 250°C were found to contain gal-
lium and arsenic oxides. Arsenic oxide was also present
in the films grown using DPGC, even at temperatures
too low for GaAs dissociation. It is well known that the
formation and stabilization of metastable high-temper-
ature phases during the thermal decomposition of MO
compounds may be responsible for the enhanced cata-
lytic activity of the solid phase in the decomposition of
MO compounds and secondary transformations of
ligands and organic compounds. Clearly, the presence
of DPAC, DPGC, and DPIC in the gas phase initiates
substrate oxidation, leading to the incorporation of gal-
lium and arsenic oxides into the growing film. Without
the MO compounds, no GaAs oxidation occurs at the
same temperatures.
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Transport Properties of Gallium and Indium Oxides Pre-
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INORGANIC MATERIALS Vol. 38 No. 5 2002