Thin Solid Films 386 2001.

233238

Production of ultrafine titanium dioxide by DC

plasma jet
Seung-Min Oh, Dong-Wha Park

Department of Chemical Engineering, Inha Uniuersity, 253 Yonghyun-dong, Nam-Gu, Inchon 402751, South Korea
Received 17 June 1999; accepted 04 April 2000

Abstract
A thermal plasma jet has been used for the synthesis of ultrafine TiO2 . As source material, TiCl4 was
injected with vapor phase by Ar-carrier gas and with liquid drop by micro pump. Particle compositions were
observed for reactor configuration, collecting position, plasma power, and various flow rates of raw
material, respectively. The characteristics of the powder such as particle size, size distribution, and phase
composition were analyzed with XRD, SEM, TEM, EDS, DTA and particle size analyzer. When TiCl4 was injected
with the vapor phase, the rutile content of the powder increased with the flow rate of Ar-carrier gas and
input power. In the case of injecting liquid phase TiCl4 , particle compositions were not affected by the flow
rate of TiCl4. Most of the powder was mainly composed of anatase. However, the powder obtained on the Atype reactor wall was observed with 95% rutile. Also, we have investigated the phase transformation
phenomena of anatase-to-rutile. After heat treatment, the anatase-to-rutile transformation started at
approximately 600C and completed at 1000C. The size of the powder and particle agglomeration
depended on the flow rate of TiCl4 and quenching gas. Most of the powders were white-colored and their
average diameter increased from 20 to 300 nm according to the flow rate of TiCl4. 2001 Elsevier Science
B.V. All rights reserved.
u phun nhit plasma c s dng tng hp TiO2 siu mn. Nh ngun vt liu, TiCl4 c cho vo
pha kh bi bnh ng kh Argon v dung dch ri bi my bm. Hp cht ht c xt h l phn ng, v tr thu
sn phm, nng lng plasma, v tc dng khc nhau ca vt liu th, ln lt. Nhng tnh cht ca bt
nh kch thc ht , kch thc phn b, v pha hn hp c phn tch vi XRD, SEM, TEM,EDS, DTA v my
phn tch kch thc ht. Khi TiCl 4 c cho vo vi pha hi, hm lng rutin ca bt tng theo tc thi ca
kh Ar v ngun nng lng vo. Trong trng hp a vo pha TiCl 4 lng, ht ca hn hp khng b nh hng
bi tc thi ca TiCl4. Phn ln bt ch yu c to ra l anata. Tuy nhin, bt thu c trn bung phn
ng A c ti 95% rutin. Cng v th, chng ti nghin c hin tng chuyn i pha t anata sang rutin.
Sau khi c gia nhit, qu trnh chuyn i t anata sang rutin bt u nhit sp x 600 oC v hon thnh
1000oC. Kch thc ca bt v ht thiu kt da vo tc thi TiCl 4 v kh lm ngui. Phn ln bt c mu
trng v ng knh trung bnh t 20 n 300nm da theo tc thi TiCl 4.
Keywords: Titanium dioxide; Thermal plasma; Phase transformation; Ultrafine powder

1. Introduction
Titanium dioxide has been used in wide
applications such as an opacifier [1], catalyst
support [2], and semi- conductor [3] due to
its superior properties with regard to chemical
stability, high permitivity and refractivity,

[4]. Recently,
and optical
transmittance
developments
have led to the use of titanium dioxide as
a photocatalyst in the removal of organic matter from
wastewater streams [5]. In these applications the
particle morphology, size distribution, and phase
composition are
key characteristics, which must be controlled
[6].
Oxit titan c s dng rng ri trong nhiu
ng dng nh thit b bo v [1], h tr xc
tc[2], bn dn [3] bi v s n nh ha hc tt,
hng s in mi, tnh khc x v h s truyn
cao [4]. Gn y, nhng s pht trin dn ti
vic s dng titan oxit nh xc tc quang
loi b cc thnh phn hu c khi dng nc
thi.[5] Trong nhng ng dng ny, hnh dng
ht, kch thc phn b, v pha kt hp l
nhng tnh cht quyt nh, cn phi c kim
sot.[6]
Titanium dioxide powders are commonly
produced by two processes: the sulfate and
chloride processes [7]. The chloride process is
regarded as the more modern
Bt titan oxit thng c sn xut bi 2 qu
trnh: qu trnh sunfat v qu trnh clo. Qu
trnh Clo thng c s dng v n hin i
hn
.

Corresponding author. Tel.: +82-32-860-7468; fax:

+82-32-872- 0959.
E-mail address: dwpark@inha.ac.kr D. Park..

process, which was initially used by Du Pont

for pro- ducing high-purity rutile [1]. In this
process, TiCl4 and oxygen along with various
additives react to form TiO2 powder by
burning a fuel, or directly heating the reactant.
, n c s dng u tin bi Du Pont cho sn
xut ruitn c tinh khit cao [1]. Trong tin
trnh ny, TiCl4 v oxi cng vi cc ph gia
khc nhau phn ng vi dng bt TiO2 bi t
cht nhin liu hay trc tip nung phn ng.
In addition, it has been reported that
titanium dioxide powders produced in thermal plasmas
without additives are predominantly anatase [8]. The
introduction of AlCl3 to the thermal plasma
process increases the
[9]. The high temperature in
amount of
rutile
the
thermal plasma reactor leads to shorter
processing times, which translates into a
relatively
smaller
reactor
with
high
throughput. The main benefit of this process
for synthesizing ultra-fine powder includes an
environ- mentally
cleaner process
with
decreased emissions of waste gases, and the
potential to produce high quality powders in
one step. In this case, the rapid quench
downstream of the hot zone induces supersaturation of the dissociated precursor vapor,
which in turn leads
Thm vo , c bo co cho rng bt oxit
titan c sn xut bi nhit plasma m khng
c cht ph gia s ra ch yu l pha anata.[8]
S c mt ca AlCl3 trong tin plasma lm
tng lng ln rutin.[9] Nhit cao ca l
phn ng plasma dn n thi gian tin trnh
ngn i, lm chuyn cho l phn ng nh hn
tng ng vi mc tiu th cao.
Li ch ch yu ca qu trnh tng hp bt mn
bao gm tin trnh lm sch mi trng vi
vic gim cht thi kh, v kh nng sn xut
bt cht lng cao trong mt bc. Trong
trng hp ny, sn phm lm lnh nhanh ca
vng nng bao gm hi trc phn ly siu bo
ha,

0040-6090/01/$ - see front matter 2001 Elsevier Science B.V. All

rights reserved. PII: S 0 0 4 0 - 6 0 9 0 0 0 . 0 1 6 4 8 - 5

23
4

S.-M. Oh, D.-W. Park / Thin Solid Films 386

(2001) 233238

to the desired chemistry and to the

formation of fine powder via homogenous
nucleation [10]. The powder is collected in the
water-cooled collection chamber and in a filter
attached to the outlet of this chamber. However, the kinetics of formation of rutile and
anatase from oxidation of TiCl4 are far from
being fundamen- tally understood, especially
for the case of no additives [11].
Ci m tr thnh ham mun ha hc v dn
n hnh dng ca bt mn qua s to mm
ng th [10]. Bt thu c trong bung thu
c lm lnh bng nc v trong ch lc nh
bn ngoi bung. Tuy nhin, ng nng ca s
hnh thnh rutin v anata t qu trnh oxi ha
TiCl4 i kh xa so vi hiu bit c bn, c bit
trong nhng trng hp khng c cht ph gia
[11].
The purpose of this study is to develop a
plasma process for preparing ultra-fine TiO2 .
Consequently, we have tried to investigate
the effects of various parameters on powder
morphology, size, size distribu- tion and
phase composition of the powder synthesized
by oxidation of
in a DC plasma jet. Also,
TiCl4
the
phase transformation of TiO2 powder has been
investi- gated. Therefore, we determined
detailed operating conditions for controlling
various characteristics of the powder.
Mc tiu ca nghin cu ny l pht trin tin
trnh plasma cho chun b TiO2 mn. V vy,
chng ti c gng tm ra nhng thng s khc
nhau nh hng n hnh thi bt, kch thc,
kch thc phn b v pha hp thnh ca bt
c tng hp
2. Experimental
2.1.

Thermodynamic calculations
Firstly, chemical equilibrium compositions in
various systems were calculated using a
software program based on Gibbs free energy
[12].
minimization
These
chemical
equilibrium calculations are not exactly
correct, but the results are useful for
preliminary experiments [13]. Fig. 1 shows
the results of calculations for different
molar ratios of TiCl4/O2 . In the
temperature range
from 1000 to 2600 K, condensed product
consists only
of TiO2 . Therefore, it was considered that
TiCl4 vapor collided with reactant oxygen,
thereby forming titanium oxy-chloride and
TiO2 . Chlorine, the gaseous reaction product,
significantly dissociates above 1500 K. The

significant effect on the reaction kinetics [14].

However,
unreacted
titanium
chloride
remained in a wide range of temperature as
shown in Fig. 1a. As the amount of oxygen
reactant is increased, the titanium oxychloride and TiCl n radicals decrease as shown
in Fig. 1b. Excess oxygen tends to increase the
ClO present in the system and decrease the Ti
oxy-chlorides as well as TiCl n radicals.
According to these results, oxygen was injected excessively to increase the conversion.
Mt tc ng mnh ln ng nng phn ng
[14]. Tuy nhin, TiCl4 cha phn ng cn li
trong khong ln nhit nh hnh 1a. Bi v
mt lng oxi phn ng tng, titan oxi clo v
TiCl gc gim nh hnh 1b. Oxi c xu hng
tng ClO hin ti trong h thng v gim TiClO
cng nh TiCl gc. Theo nh kt qu , oxi c
a vo nhiu tng s chuyn ha.
2.2. Experimental apparatus

A schematic diagram of the experimental

apparatus
is shown in Fig. 2. This system mainly
consisted of a
plasma torch, two types of reaction tubing
type a, hot wall; type b, water-cooled cold
wall., a quench chamber and an evacuation
system. Experiments have been car- ried out
by changing conditions such as the plasma
power, configuration of reactor, flow rate and
injecting position of reactant or quenching
gas. The plasma torch was typically ran at 8
15 kW input power with a flow rate of 15
l/min of Ar. Titanium tetrachloride TiCl4 ,
99.9% purity, Aldrich Co.. was used as a source
material. This was fed and controlled by two
methods. Firstly, liquid phase TiCl4 was
injected into the plasma flame with a flow rate
of 0.54.3 g/min by a micro pump.
Alternatively, TiCl4 vapor was introduced into
the plasma flame by an Ar-carrier gas. The
Ar-carrier gas was injected at 1.56.0 l/min,
then a practical flow

was measured from 0.1 to 0.2

rate of
g/min.
TiCl4
dissociation and re-association of chlorine may
have a
u tin, nhng hp phn cn bng ha hc
trong nhiu h thng khc nhau c tnh ton
bng cch s dng chng trnh phn mm da
trn s gim nng lng ca Gibb [12]. Nhng
tnh ton ny khng hon ton chnh xc, nhng
kt qu l c ch cho nhng th nghim s b

S.-M. Oh, D.-W. Park / Thin Solid Films 386

(2001
[13]. Hnh 1 cho thy kt qu
ca) 233238
tnh ton cho
t l mol khc nhau ca TiCl4/O2. Trong khong
nhit t 1000 n 2600 K, sn phm ngng
t ch gm TiO2. V th, n c xem rng hi
TiCl4 va chm vi oxi phn ng, bng cch y
to nn titan oxi clo v TiO2. Kh Clo v sn
phm kh phn ng hon ton phn ly khi trn
1500 K. S phn ly v ti kt hp ca Clo c
th c

23

5
Reacting and quenching gases were injected
through
the anode nozzle, at the top of the reaction
tube, and the quenching gas injection port of
the
quench
chamber,
respectively.
Evacuated gases were passed through a bag
filter and a scrubber by a vacuum pump.
The detailed experimental conditions are
given in Table 1.
Biu v nhng thit b th nghim c th
hin hnh 2. H thng ny ch yu bao gm
u plasma, hai loi phn ng ng Z loi a,
tng nng; loi b, tng lm lnh bng nc,
bung lm ngui, h thng chn khng.
Nhungwex th nghim c tin hnh bng
nhng iu kin thay i nh nng lng
plasma, hnh dng l phn ng, tc dng v
v tr a cc cht phn ng hay kh lm ngui
vo. u plasma thng c chay 8-15kW
vi tc 1/min Ar. TiCl4 tinh khit 99.9%
ca Cng ty Aldrich c s dng nh vt liu
ngun. N c cho vo v kim sot bi 2
phng php. u tin, pha dung dch TiCl4
c a vo ngn la plasma vi tc 0.54.3g/m bi my bm. Thay v vy, hi TiCL4
c dn vo ngn la plasma bi kh Ar ng
hnh. Kh Ar ng hnh c a vo 1.5-6.0
l/min, sau tc dng thc t ca TiCl4
c tnh t 0.1 n 0.2 g/min. Kh phn ng
v lm ngui c vo qua u anot, u ca
ng phn ng, v cng a kh lm ngui vo
ca bung lm ngui tng ng. Kh chn
khng c chuyn qua ti lc v thit b lc
bi my bi chn khng. Chi tit iu kin th
nghim c cho bng 1.

Fig. 1. Chemical equilibrium compositions in different molar ratios. a. TiCl4/O2 = 1:1 b. TiCl4/O2 = 1:4.

Table 1
Experimental conditions for plasma synthesis

Input power
Plasma gas flow rate
Reaction tube
dimension
TiCl4 feeding rate

815 kW
15 l/min
A-type: I.D., 35 mm, L, 40 mm
B-type: I.D., 45 mm, L, 400 mm
0.10.2 g/min
Ar-carrier gas: 1.56.0
l/min. 0.54.3 g/min
520 l/min

Oxygen flow rate

2.3. Characterization of synthesized powder

Synthesized powders were collected in the
reaction tube, quench chamber, and filter,
respectively, and they were investigated for
their phase compositions using an
Model PW 1710, Philips Co...
X-ray
diffractometer
The rutile content was calculated using the
following equation [15]:
Bt tng hp c thu trong ng phn ng,
bung lm ngui, v lc, tng ng, chng
c phn tch thnh phn pha bng nhiu x
k tia X. Hm lng rutin c tnh bng
phng trnh sau [15]:
fR = 1 1 +
1.26 IR/IA
where fR

Fig. 2. Experimental DC plasma apparatus for preparing

ultra-fine titanium dioxide.

.
1

is the fraction of the rutile phase, IR is the

intensity of the 110. reflection of the rutile

phase and
IA is the intensity of the 101. reflection of
anatase. A drop sample was dispersed in
methanol and analyzed using a TEM/EDS
Model CM 200, Philips. by placing onto a Cu
grid. Also, the characteristics of the powder
were observed using SEM Model S-4200,
Model
Hitach.,
DTA
DTA
1600,
TA
.
Instruments , and a particle size analyzer
Model SYS 4700, Malvern Instrument Co...
3. Results and discussion
3.1. Phase compositions of the
synthesized from TiCl4 uapor

powders

Fig. 3 shows the X-ray diffraction patterns of

the powder synthesized under the following
conditions: 8 kW of plasma input power; 2
l/min of Ar-carrier gas for injecting TiCl4
vapor; and 5 min of operating time. The
powder obtained on the A-type reactor was
esti- mated to be composed of 80% rutile and
20% anatase as shown in Fig. 3a. Compared
with the powder heat treated at 800C Fig.
3d., the powder in a. appeared to have a

higher rutile content. It was thought that the

radiation heat of the plasma jet flame affected
the powder in the A-type reactor. The XRD
pattern of the powder obtained from the B-type
reactor corresponded to anatase Fig. 3b.. The
line broadening should be due to the fine size
and amorphous state of the powder and it
resulted from rapid quenching by a watercooled reactor wall.
Hnh 3 cho thy vn nhiu x tia X ca bt
tng hp di nhng iu kin sau: 8kW nng
lng plasma u vo; 2 l/m kh Ar ng hnh
thm hi TiCl4; v 5 pht hot ng. Bt
nhn c trong l phn ng A vo khong 80%
rutin v 20% anata nh hnh 3a. So snh vi bt
c gia nhit 800oC hnh 3d th bt A c
hm lng rutin cao hn. iu c ngha l
nhit bc x ca ngn la plasma nh hng
n bt l A. Hnh nh XRD ca bt thu c
t l B cho anata hnh 3b. ng m rng l bi
v ht mn v trng thi v nh hnh ca bt v
n l kt qu t vic lm lnh nhanh bi nc.
Fig. 4 shows the rutile content of the powders
calcu- lated as a function of the flow rate of
Ar-carrier gas, when the powders were
synthesized in the B-type reac- tor. The rutile

content increased with the input plasma

power, but there was no significant change
over 12 kW
of input power. The rutile content increased by
up to60% with a flow rate for Ar-carrier
gas of 1.56.0
l/min. Then, the flow rate of TiCl4
was
estimated from
0.1 to 0.2 g/min. From these results, it was
considered
that the reaction temperature of TiCl4 vapor
increased with increasing flow rate of the Arcarrier gas
Hnh 4 cho thy hm lng rutin ca bt c
tnh nh chc nng ca tc ca kh ng
hnh Ar, Khi bt c tng hp trong l B.
Hm lng rutin tng vi nng lng plasma
u vo, nhng ko c s thay i nhiu khi
nng lng trn 12kW. Hm lng rutin tng
ln ti 60% vi tc dng Ar 1.5-6.0 l/min.
Khi , tc dng ca TiCl4 c c tnh t
0.1-0.2 g/min. T nhng kt qu, n c xem
xt l nhit phn ng ca hi TiCl4 tng
vi s tng tc dng Ar.

In
Fig.
3ce,
anatase
to
rutile
transformations were shown for the heattreated powder at 600, 800 and 1000C for 2
h, respectively. Phase transformation of the

powder started at approximately 600C and

com- pleted at approximately 1000C. Also, it
was observed
Trong hnh 3c-e, s chuyn i t anata ti
rutin c th hin cho nhit bt 600, 800
v 1000 C trong 2 gi, tng ng. S
chuyn i pha ca bt bt u sp x 600
C v hon thnh gn 1000 C. V th, n
c xt

Fig. 3. X-Ray diffraction patterns of the powders obtained

at differ- ent positions and after heating of b.. a. A-type
reactor; b. B-type reactor; c. 600C; d. 800C; and e.
1000C.

diameter of the powder increased from 20 to

300 nm with heating temperature. Also, the
shape of the powder changed from spherical to
tetragonal structure due to crystal growth.
Rng nhit ta ra ngoi bi v s chuyn i pha
c chuyn i trn 500 C t ng cong
DTA. Hnh thi ca bt c xem xt vi SEM
nh hnh 5. In-situ bt tng hp trong hnh 3b
cho thy ng knh khong 20nm nh hnh 3a.
ng knh trung bnh ca bt tng t 20 n
300nm vi nhit nung. V th, hnh dng ca
bt thay i t hnh cu sang cu trc bt gic
bi v tinh th pht trin.
3.2.

Fig. 4. Rutile content as a function of flow rate of Arcarrier gas for TiCl4 .

that the exothermic heat due to phase

transformation was generated over 500C
from the DTA curve. The morphology of the
powders was observed with SEM as shown in
Fig. 5. In situ powder synthesized in Fig. 3b
was well distributed with a diameter of
approximately 20 nm Fig. 3a.. The average

Phase compositions of the powder

synthesized from liquid phase TiCl4

When the raw material was fed with liquid

phase TiCl4 by micro pump, the resulting
powders gave X-ray diffraction patterns as
shown in Fig. 6. The powders were obtained
at different collecting positions: a. fil- ter; b.
quench vessel; c. B-type reactor wall; and d.
A-type
reactor
wall,
respectively.
The
plasma-input

Khi nguyn liu th c cho vo vi pha

lng TiCl4 bi my bi, kt qu nhiu x tia X
cho bt c th hin hnh 6. Bt thu c
nhiu v tr thu hoch a. lc, b. bung lm
ngui, c. bung phn ng loi B v d. bung
phn ng loi A, tng ng..

Fig. 5. SEM photographs of the powder heat-treated at:

a. in situ;
b. 600C; c. 800C; and d. 1000C.

Fig. 6. X-Ray diffraction patterns of the powder collected

at differ- ent positions TiCl4 flow rate = 1.5 g/min.. a.
Filter; b. quench vessel; c. B-type reaction tube; d. Atype reaction tube.

power was 8 kW and the TiCl4 liquid was fed

at a flow rate of 1.5 g/min. The main peak of
the powder obtained at a., b., and c.
corresponded with anatase, probably due to
rapid quenching by the water-cooled reaction
tube wall. The powder obtained in the A-type
reactor
wall
showed
a
sharp
peak
corresponding with rutile. The rutile content
was calculated to be over 95%. It was
considered that the higher rutile content was
due to radiation heat from the plasma jet
flame. The weight percentage of the powders
for
different
collecting
positions
were
estimated at approximately 25% a., 10% b.,
20% c. and 20% d., respectively, and
weight loss was calculated at 25%.
Nng lng plasma u vo l 8kW v dung
dch TiCl4 c a vo tc 1.5 g/min.
nh ch yu ca bt thu c a, b, v c
tng ng vi anata, c l bi v lm lnh
nhanh bi nc lnh ng phn ng. Bt thu
c trong l phn ng loi A cho thy nh
nhn tng ng vi rutin. Hm lng rutin c
tnh trn 95% N dduocj xem xt rng hm
lng rutin cao l bi v nhit pht t ngn la
plasma. Phn trm khi lng ca bt v tr
thu hoch khc nhau c c tnh sp x 25%
a, 10% b, 20% c, 20% d, tng ng, v
khi lng mt i khong 25%.

3.3.

Morphology of the powder

Powder morphology was observed
for
various flow rates of TiCl4 from 0.2 to 1.5
g/min as shown in Fig. 7. The powder of a.
was synthesized by injecting vapor phase
TiCl4 , while others were synthesized by
injecting liquid phase TiCl4 . The mean particle
diameter was estimated to be within a narrow
range of 30100 nm at a flow rate below 0.5
g/min [a. and b.]. The size of the powder
was the same from each position: B-type
reactor, quench chamber and filter. There
was better growth and agglomeration of the
powder with increas- ing flow rate of TiCl4 , as
shown in Fig. 7. For the powder obtained on
A-type reactor wall, it was partly sintered by

plasma radiation heat and had an approximate average diameter of 200 nm. Fig. 8
shows a TEM photograph of the powder
synthesized as follows: 8 kW
Hnh thi ca bt c xt cho nhiu tc
dng TiCl4 khc nhau t 0.2 n 1.5 g/min th
hin hnh 7. Bt a dduocj tng hp bng
cch a pha hi TiCl4., trong khi bt khc
c tng hp bi pha TiCl4 lng. ng knh
thc c tnh trong khong hp 30-100nm
tc dng di 0.5 g/min [a v b]. Kch thc
ca bt l bng nhau t tng v tr: l B, bung
lm ngui, v lc. Ta c s pht trin tc hn
v s ng t bt vi s tng tc dng
TiCL4 nh hnh 7. Cho bt thu dduocj l A, n
b thiu kt tng phn bi nhit plasma pht ra
v ng knh trung bnh khong 200nm. Hnh
8 cho thy nh TEM ca bt tng hp theo
sau: 8kW
The flow rate of quenching gas affected the
particle size distribution as shown in Fig. 9.
The particles were well distributed with
increasing flow rate of quenching gas, but the
phase composition remained constant. Also
there was greater agglomeration of particles at
lower flow rates of the quenching gas.
Tc dng lm ngui nh hng ti kch
thc ht nh trong hnh 9. Ht c phn tn
tt vi s tng tc dng lm ngui, nhng
pha hn hp cn li gi nguyn. V th s ngng
t ht cao hn tc dng lm ngui thp.

Fig. 7. SEM photographs of the powder at different flow

rates of TiCl4 : a. 0.2 g/min by TiCl4 vapor.; b. 0.5
g/min; c. 1.0 g/min;
d. 1.5 g/min.

of plasma input power and Ar-carrier gas at a

flow rate of 4 l/min. The powder was
observed to have an approximate diameter of
30 nm composed of 33.5% titanium and
66.5% oxygen from TEM/EDS analysis. The
other peaks in Fig. 8b were due to the
carbon- coated Cu grid used for placing
sample powder.
Nng lng plasma u vo v kh Ar ng
hnh tc 4 l/min. Bt c xt c ng
knh khong 30nm gm 33.5% titan v 66.5%
oxi qua phn tch TEM/EDS. Nhng nh khc
hnh 8b l bi v li Cu ph cacbon c s
dng thay th mu bt.

Fig. 9. SEM photographs of the powder at different flow

rates of the quenching gas: a. no flow; b. 10 l/min.

powder obtained on the A-type reactor was

80%, re- gardless of the flow rate. It
increased from 10 to 60% with the flow rate
of Ar-carrier gas on the B-type reactor. The
reason for this was that the powder was
affected by radiation heat from the plasma
jet flame containing rutile in the A-type
reactor. Also, it was observed that TiCl4 vapor
reacted in the higher tem- perature region
of the plasma with increasing flow rate of the
Ar-carrier gas. Rutile content increased with
plasma power but it did not change
significantly beyond 12 kW of input power.
4. Conclusions
We have concluded the following results.
Reaction

The average particle diameter increased from

20 to 300 nm according to the flow rate of
TiCl4 .
bt thu c trn bung phn ng A l 80%
theo tc dng. N tng 10-60% vi tc
dng Ar trn bung phn ng B. L do cho vic
ny l do bt b tc ng bi nhit pht t
ngon la plasma gm rutin trong bung A. V
th, n c xt rng hi TiCl4 phn ng trong
vng nhit cao hn ca plasma vi s tng
tc dng ca Ar. Hm lng rutin tng vi
nng lng plasma nhng n khng thay i
nhiu sau 12 kW. ng knh ht trung bnh
tng t 20 n 300nm theo tc dng TiCl4
When liquid phase TiCl4 was injected by
micro pump, most of the powder obtained
from the B-type reactor was converted to
anatase showing a white-color, whereas the
powder obtained in the A-Type reactor was
mainly composed of rutile > 95%.. The
powder obtained from the A-type reactor was
partly sintered by radiation heat from the
plasma jet flame and its size was estimated
to be 200 nm. At another position, it was
estimated to be dozens of nanometers at a
lower flow
rate of TiCl4 below 1.0 g/min and it
increased with
increasing flow rate of TiCl4 .
Khi pha lng TiCl4 c thm vo bi my bi,
phn ln bt thu c t B b chuyn thnh
anata c mu trng, trong khi bt thu c
trong A ch yu gm rutin >95% Bt thu t A b
thiu kt tng phn bi nhit pht ra t ngn
la plasma v kch thc ca n khong 200nm.
v tr khc n c th khong 12 nm dng
thp.
Acknowledgements

positions and the injection method of affected

TiCl4
vap
the characteristics of the powder.
or
When TiCl4
was injected as raw material, the rutile
content of the
Chng ta kt lun theo kt qu sau. Nhng v
tr phn ng v phng php a vo ca TiCl4
nh hng n tnh cht ca bt Khi hi TiCl4
c a v nguyn liu th, hm lng rutin
ca

This work was supported by grant No.

981-1106-1
Fig. 8. TEM photograph and EDS analysis of the powder
obtained in Fig. 7a.

from the Basic Research Program of the

KOSEF.
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