1D-6-32

Preparation of thick PZT film by electrostatic spray deposition (ESD)

for the application in micro-system technology

Jian Lu, Jiaru Chu’, Wenhao Huang, Zhimin Ping

(Dept. of Precision Machinery and Instrum., Univ. of Sci. and Tech. of China, 230027, Hefei, China)

As one of the most useful functional materials, PZT (Pb(Zrx,Ti,J03) films are of
great interest in micro-systems for the fabrication of microsensors and microactuators.
Among the methods for preparation of PZT films, such as sol-gel, laser ablation,
sputtering and jet molding, it is difficult to obtain good piezoelectric properties and
high film thickness at the same time. In this paper, we introduce a new deposition
method for thick PZT film preparation, named “electrostatic spray deposition (ESD)”,
using sol-gel solution as precursors. It offers the advantages of high film growth rate,
easy control of film compositions, simple setup and low cost. Electrostatic spray was
studied theoretically by Rayleigh“] and was deep investigated by A.Gomez and Keqi
Tang [*I. C.H.Chen et al. applied electrostatic spray to ceramic film deposition [31.Our
results proved that it is a promising method for thick PZT film preparation with
relatively good piezoelectric properties.
The configuration of our experimental setup is shown in Fig 1 . The electrostatic
spray system is comprised of a precursor feeding unit, a stainless steel capillary and a
ground electrode. With a heater and a thermal couple, the wafer’s temperature can be
well controlled. Steady electrostatic spray mode, named “cone-jet mold”, is shown in
Fig. 2. The spray angle was estimated about 100 degrees, which means large
deposition area coverage. It was found that the higher the applied electric potential or
the liquid flow rate is, the larger the spray angle is with given precursor liquid and
geometry of the electrostatic spray system. Fig. 3 (a) shows the XRD patterns for 100
nm thick sol-gel PZT film prepared on bottom electrode Pt. Fig. 3 (b) and (c) show
the XRD patterns for ESD PZT films deposited on Pt and on 100 nm thick before
annealed sol-gel PZT/Pt, respectively. It revealed that the film consist of only the
pervoskite phase. The film deposited by ESD on Pt shows no preferred orientation,
while the film that deposited on l00nm thick before annealed sol-gel PZT/Pt exhibits
preferred strong PZT (100) orientation. It indicates that the use of sol-gel PZT as
intermediate layer affected as-deposited film’s nucleation and growth behavior and
enhanced the film’s orientation. The films shown in Fig. 3 (b) and (c) were deposited
for 10 minutes (baking at 350°C for l h and 600°C for 20 minutes after each 5
minutes deposition) at normal temperature and 1 micron thickness were obtained. It
indicated that 500 nm thick PZT films can be achieved in each layer, which is proceed
to sol-gel method. Because sol-gel method can only achieve about 100 nm per layer in
thickness, otherwise it will crack when sintered at high temperatures. Fig. 4 shows the
surface morphology of PZT films deposited by ESD. The film was optically clear and
uniform.
Preparation of PZT films by ESD at different substrate temperatures was also
conducted. We found that high deposition temperature result in PZT (1 10) orientation
and highly porous morphology. It is difficult to achieve good piezoelectric properties
at high deposition temperature. The experimental processes and other results will be
presented in details in this paper.
Reference:
[ I ] Lord Rayleigh, “On the equilibrium of liquid conducting masses charged with electricity”, Philos.
Mag., 14,184(1882)
[2]A.Gomez and Keqi Tang, “Charge and fission of droplets in electrostatic spray”, Phys. Fluids,
6( l), 1994
[3]C.H.Chen, M.H.J.Emond, E.M.Kelder et al., “Electrostatic sol-spray deposition of nanostructured
ceramic thin films”, J.Aerosol Sci., 30(7), 1999

‘Corresponding author, Fax: +86-551-3607107, Email:jrchu:ijiustc.ctlu.cn

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Fig 1 The schematic view of the electrostatic Fig 2 The cone-jet spray mode
spray deposition system (Applied Voltage: 4500V Flow rate:0.6ml/h)

m
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0- j,L, , , , , .
8 4000-

20000 -
10000 1 PV(110)
0- 1 , I . . ’ . . , r

15 20 25 30 35 40 45 i0 55 60
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Fig 3 XRD patterns for PZT films after annealing at 600’C Fig 4 Crack free PZT film deposited by electrostatic
for 4 hours (a)100 nm thick sol-gel PZT on Pt (b) spray method
10 minutes ESD PZT on Pt (c)10 minutes ESD PZT
on 100 nm thick before annealed sol-gel PZT/Pt

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