Journal of Materials Processing Technology 209 (2009) 58865891

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Journal of Materials Processing Technology

journal homepage: www.elsevier.com/locate/jmatprotec

Rapid fabrication of alumina-based ceramic cores for gas turbine blades by

stereolithography and gelcasting
Haihua Wu, Dichen Li , Yiping Tang, Bo Sun, Dongyang Xu
State Key Laboratory of Manufacturing Systems Engineering, Xian Jiaotong University, Xian, Peoples Republic of China

a r t i c l e

i n f o

Article history:
Received 15 November 2008
Received in revised form 12 May 2009
Accepted 3 July 2009

Keywords:
Alumina-based ceramic core
Stereolithography
Gelcasting
Drying shrinkage
Sintering shrinkage

a b s t r a c t
Injection moulding is accepted as one of the most important methods for shaping complex ceramic
cores, which are used to form intricate internal cooling passages of gas turbine blades. But the relatively
long lead time and high costs involved in the fabrication of hard tooling render it uneconomical for
new products development and low-volume production. In the study, a rapid prototyping process is
developed to fabricate complex-shaped alumina-based ceramic core by combining stereolithography
(SL) with gelcasting. SL is utilized to fabricate an integral sacricial resin mold, and gelcasting is utilized
to form a wet ceramic core green body through polymerization of aqueous ceramic slurry. The freezedrying process is adopted to treat the wet green body surrounded by the resin mold, the drying shrinkage
is decreased, and the generation of crack can be prevented. The sintering shrinkage of ceramic core is
controlled by adding magnesium oxide power and developing a novel sintering process. After the resin
mold is burnt out, the complex-shaped alumina-based ceramic core is obtained.
2009 Elsevier B.V. All rights reserved.

1. Introduction
In investment casting, ceramic cores are used to form intricate
internal cooling passages of gas turbine blades, they are mainly fabricated by injection moulding (Ford, 1997). The injection moulding
process involves a number of successive operations: metal die fabrication, slip preparation, moulding, demoulding, binder removal,
sintering, monitoring and additional operations. To obtain a lowviscosity slip with good formability and provide a green body with
sufcient strength, a considerable amount of binder (up to 1420%
by mass) is added to mix with ceramic powders, which makes the
subsequent binder removal difcult, a slow heating process (spending 48 h or more) is adopted to avoid warping or cracking. To extract
the green body from the metal die without damaging ceramic cores,
metal die is often divided into several movable pieces, which needs
many design skills. Because there are many repeated modications
to the design, it often takes 1525 weeks and several or 10,000 dollars to fabricate a set of complex metal dies (Dunne et al., 2004).
Injection moulding is not suitable for new products development
and low-volume production, due to the time consuming and expensive hard tooling development and the relatively long time for
binder removal.

Corresponding author at: State Key Laboratory of Manufacturing Systems Engineering, Xian Jiaotong University, Xian, Peoples Republic of China.
Tel.: +86 29 82665575; fax: +86 29 82660114.
E-mail address: xjtudcli@sina.com (D. Li).
0924-0136/$ see front matter 2009 Elsevier B.V. All rights reserved.
doi:10.1016/j.jmatprotec.2009.07.002

Gelcasting, an advanced and near-net-shape ceramic forming

process, is developed to overcome some of the limitations of
other forming processes such as injection molding and slip casting
(Omatete et al., 1997). Compared with injection moulding, gelcasting is much simpler and more suitable for single piece and small
volume production. Gelcasting uses only small amount of organic
binder (only 34% by mass), and does not need the critical binder
removal step. The green body has a high exural strength, because
there is plenty of three-dimensional network polymer in the green
body. Gelcasting molds are non-porous molds, a variety of mold
materials such as metals, glass, wax and plastics can be used. This
means that molds of very complex shapes can be made from inexpensive materials. The aqueous ceramic slurry has low viscosity and
can ll up mold cavities with ease, the complexity of shape attained
by gelcasting is limited only by the ability of mold design (Cai et al.,
2003; Vandeperre et al., 2003).
Limitations on ceramic core shape and volume imposed by
difculties of metal die preparation may be overcome by rapid
prototyping process. Stereolithography (SL) is a typical rapid prototyping process and has the capability of rapidly fabricating any
complex-shaped resin prototypes which have high forming accuracy, good rigidity and ne surface quality. In the low-volume
production, the metal molds are replaced by the resin prototypes to
dramatically reduce the cost and lead time. SL prototypes have been
successfully used as low-pressure molds for complex ceramic parts.
In investment casting, the SL prototypes have been successfully
used to substitute wax patterns to fabricate multi-layer ceramic
shells (Tay et al., 2003; Cheah et al., 2005; Onuh and Hon, 2001).

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Fig. 1. (a) CAD model and (b) the resin mold fabricated by SL.

In the study, a novel rapid prototyping process is presented

and developed to fabricate complex alumina-based ceramic cores
by combining SL with gelcasting. First, an integral sacricial resin
mold rapidly fabricated by SL is used to replace the metal die,
and injection moulding is substituted by gelcasting to fabricate
complex-shaped ceramic cores. Aqueous ceramic slurry is cast into
the resin mold and in situ polymerized to form a wet ceramic core
green body, of which all parts are connected together. To keep
the structural integrality of complicated ceramic core, the drying
shrinkage of the green body is minimized by freeze drying, and a
novel sintering process is adopted to reduce the sintering shrinkage.
2. Fabrication of alumina-based ceramic cores
2.1. Resin mold preparation
In the study, the resin mold made of Somos14120 resin from DSM
Corporation was designed as an integral one, which can be removed
by pyrolyzing in the subsequent sintering process. The die parting
face and demoulding step were eliminated, so it is possible to obtain
very complicated components within the resin mold (Lindqvist and
Carlstrm, 2005).
The resin mold preparation was as follows: rst, CAD model,
with the negative of the desired ceramic core, was designed using
PRO/E software, and then it was converted into STL format and
sliced into layers with a thickness of 0.05 mm through dataprocessing software; nally, the resin mold was fabricated quickly
and automatically using the SL apparatus SPS 450B developed by
the Institute of Advanced Manufacturing Technology in Xian Jiaotong University of China, and the resin mold fabricated by SL is
shown in Fig. 1, it has intricate structures and is difcult to fabricate
with traditional manufacturing methods. In order to pour aqueous
ceramic slurry into the mold smoothly, a bottom gating system was
designed.
2.2. Slurry preparation
The ner and coarser alumina powders (D50 = 5 m and
D50 = 25 m, 99.32%) supplied by Shandong Zibo Aluminum Inc.

were chosen as the matrix material of ceramic core, and magnesium oxide power (D50 = 2 m, 99.99%) and yttrium oxide power
(D50 = 2 m, 99.99%) supplied by Sinopharm Chemical Reagent
Co., Ltd. were used as mineralizers. Deionized water was chosen as solvent, acrylamide (CH3 CONH2 , AM) as organic monomer,
N,N-methylene diacrylamide (C7 H10 N2 O2 , MBAM) as cross-linking
agent, ammonium persulfate as initiator, N,N,N ,N -tetramethyl
ethylenediamine (C6 H16 N2 ,TEMED) as catalyst, and sodium polyacrylate as dispersant.
According to the ow chart of aqueous gelcasting process for
alumina (Ma et al., 2003; Tong and Chen, 2004), rst, a premixed
solution with the concentration of 25% was prepared by dissolving
AM and MBAM (in 24:1 ratio) in proper amount of deionized water.
The pH value of the premixed solution was adjusted to 11 by strong
ammonia after sodium polyacrylate (2.5 wt% of solid powers) was
added. Subsequently, all powders (consisted of 75% coarser alumina
powder, 16% ner alumina powder, 4% magnesium oxide powder
and 5% yttrium oxide powder by mass) mixed with low speed agitation in advance were added into the premixed solution in steps.
By ball-milling for 23 h, the ceramic slurry with low-viscosity
(0.735 Pa S) and high solids loading (55 vol.%) was prepared.

2.3. Gelcasting and drying

Vacuum deairing of the slurry can obviously improve the green
strength and reduce bubble defects (Jiang et al., 2007). After initiator and catalyst were added (1.0 wt% and 0.2 wt% of the premixed
solution respectively), the slurry was stirred in vacuum for 35 min
to eliminate air bubbles, and then the slurry was cast into the resin
mold, at the same time, a vibration (amplitude was 13 mm, vibration frequency was 3060 Hz) was applied. Induced by the initiator
and catalyst, the slurry was in situ polymerized to form a green
body. Subsequently, the green body surrounded by the resin mold
is put into the DTY-1SL Vacuum Freeze Dryer provided by Detianyou
Technology Company of China. And the deionized water was eliminated by a freeze-drying process. The actual pre-freezing time and
the sublimation time were determined by the size of the green
body.

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H. Wu et al. / Journal of Materials Processing Technology 209 (2009) 58865891

2.4. Sintering
After drying, the ceramic core green body was put into a hightemperature sintering furnace. And the sintering process is made up
of two stages. The aim of the rst stage is to burn out all organic compounds (including polyacrylamide and the resin mold). Previous
investigations show that all organic compounds come off primarily
as complete combustion products, CO2 and H2 O; the pyrolysis of the
compounds can completed below 600 C (Hague et al., 2001; Dweck
et al., 1997). The aim of the second stage is to densify the green body
and rapidly develop a certain room-temperature exural strength.
2.5. Characterizations of the specimens
According to the above-mentioned process, the specimens (
10 mm 120 mm) were prepared, which are surrounded by the
resin mold and only left two ends open. The specimens were dried
using an air-drying process and a freeze-drying process. And the
lengths of specimens were measured before and after drying to
calculate the drying shrinkage. The air-drying process includes the
following steps: (i) the green body was dried initially at high relative humidity (90%) and low temperature (25 C) for 1224 h and
(ii) after the relative humidity was reduced to around 60% and the
temperature was increased to 35 C, the green body was dried for
another 1224 h. The freeze-drying process consisted of three steps:
(i) the green body was pre-freezed at 45 C for 46 h, (ii) and
then sublimed for 1224 h under a vacuum of 1020 Pa, and (iii)
continued to resolve for 23 h at 25 C.
The effect of different material compositions and different
sintering process parameters (including sintering temperature,
holding time and heating rate) on the sintering shrinkage was
investigated. The lengths of specimens ( 4 mm 50 mm) were
measured before and after sintering, and the sintering shrinkages
were calculated.
The structure and morphology characters of the freeze-drying
and air-drying polymeric hydrogels were investigated by the BX41P Polarized Light Microscopy.
3. Result and discussion
3.1. Drying shrinkage
During the SL-gelcasting process, the demoulding operation was
eliminated, which was helpful to fabricate complex-shaped ceramic
cores, but the drying shrinkage may be obstructed by internal structure of the resin mold, which may lead to cracking in the green
body. In Fig. 2a, there is a crack in the middle of the green body
(the narrowest cross-section), because the drying shrinkage in air
is hindered by the resin mold.
Some measures should be taken to minimize the drying shrinkage and decrease ceramic core cracking. Much work has been
devoted to minimize the drying stresses and avoiding cracking during gelcasting. Some soft molds such as wax mold, polystyrene
mold and dimethylsiloxane mold, have been utilized to replace hard
molds, they are allowed to deform, and the drying stress in the
green body is relieved (Dhara et al., 2002), but the forming accuracy

Fig. 3. The air-drying shrinkage and freeze-drying shrinkage.

may be affected by the deformation of soft molds. During drying in

air, the water is eliminated by diffusing outwards and evaporating, to avoid any differential drying, drying has to be carried out
under well-controlled temperature and humidity conditions, and
the drying shrinkage is dictated by the solid loading of the slurry.
The drying shrinkage can be reduced by improving solid loading
in volume, but high solid loading has unfavorable inuence on the
viscosity of the slurry.
In the study, freeze drying was used to treat the wet green body
surrounded by the resin mold. Fig. 3 shows the drying shrinkages of
specimens. The air-drying shrinkage is about 2.0%, and the freezedrying shrinkage is only about 0.25%. The freeze-drying shrinkage
is decreased signicantly, and there is no crack in the green body
(see Fig. 2b).
During the freeze-drying process, the deionized water in the
green body was rst frozen to ice crystals, and then directly eliminated by sublimation. The solid/liquid interface tension force, one
of the main driving forces of shrinkage, no longer exists, and many
pores left by the ice crystals occupy some space (see Fig. 4a), so the
drying shrinkage is evidently decreased. But it is can be seen that
the air-drying polymeric hydrogel in Fig. 4b has formed a compact
body, the volume of the hydrogel is decreased signicantly which
leads to the shrinkage of the green body (George and Schere, 1990).
At the same time, the pores are connected with each other, which
is benecial to remove the inner water of the green body. Adopting
the freeze-drying process, the thick-section or slender green body
can be dried out in a short time.
3.2. Sintering shrinkage
3.2.1. Material compositions
Excessive sintering shrinkage may lead to high sintering stress
and forming sintering cracks in ceramic cores, and the ceramic cores
may be broken. A failure case is shown in Fig. 5a. The structural
integrity of ceramic cores has been destroyed because sintering
shrinkage is up to 2.1%.

Fig. 2. (a) Air drying: a crack. (b) Freeze drying: no crack.

H. Wu et al. / Journal of Materials Processing Technology 209 (2009) 58865891

Fig. 4. The structure and morphology characters of the freeze-drying and air-drying polymeric hydrogels.

Fig. 5. Complex-shaped ceramic cores (a) a failure one and (b) an integral one.

The sintering shrinkage can be reduced by adjusting material

compositions. Fig. 6 shows the sintering shrinkages of different
specimens with different material compositions (adding/no adding
magnesium oxide power). With the increase of magnesium oxide
power content, the sintering shrinkages of specimens decrease
from 2.1% to 0.25%. The reason is that alumina power reacts
with magnesium oxide power to form MgAl2 O4 (a polycrystalline
composition), accompanying by linear expansion (2.45%), which
compensates for some of the sintering shrinkage (Mohapatra and
Sarkar, 2007). The sintering shrinkage of specimen C containing
4 wt% magnesium oxide power is lower than that of specimen B
containing 2 wt% magnesium oxide power, since the former produces much more MgAl2 O4 . But excess MgAl2 O4 may reduce the
surface activities of the powders and hinder the sintering process.
Fig. 5b shows an integral complex-shaped ceramic core, the sintering shrinkage is only 0.25%. The results showed that the structural
integrity of ceramic cores was guaranteed by adding 4 wt% magnesium oxide power.

3.2.2. Sintering process

After material compositions of complex-shaped ceramic cores
are dened, the sintering shrinkage is mainly determined by the
sintering process. In the study, the effects of sintering tempera-

Fig. 6. The sintering shrinkages of different material compositions.

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H. Wu et al. / Journal of Materials Processing Technology 209 (2009) 58865891

Fig. 9. The curve of the sintering shrinkage at different heating rates.

Fig. 7. The curve of the sintering shrinkage at different sintering temperatures.

Fig. 8. The curve of the sintering shrinkage at different holding times.

ture, holding time and heating rate on the sintering shrinkage were
investigated. Fig. 7 shows the curve of the sintering shrinkage at
different sintering temperatures, when the heating rate is 480 C/h
and the holding time is 4 h.
It can be seen that the sintering shrinkage increased with the
sintering temperature. When the sintering temperature reaches
1600 C, the sintering shrinkage exceeds 1.0%. Excessive sintering
shrinkage may result in cracking. At 1550 C, the sintering shrink-

age is low (about 0.32%), the lower sintering shrinkage means the
higher sintering qualied rate of ceramic cores. Magnesium aluminum spinel (MgAl2 O4 , the reaction product of Al2 O3 and MgO)
may form at the range of 9001400 C, and yttrium aluminum
garnet (3Al2 O3 5Y2 O3 , the reaction product of Al2 O3 and Y2 O3 )
is produced between 1400 C and 1600 C (Mohapatra and Sarkar,
2007; Medraj et al., 2006), and the sintering temperature of ner
alumina power is usually higher than 1500 C. Considering the sintering shrinkage and the sintering temperatures of different solid
powers, 1550 C is chosen.
Fig. 8 shows the curve of the sintering shrinkage in different
holding times (as the sintering temperature is 1550 C and the heating rate is 480 C/h). It can be seen that the sintering shrinkage is
increased with holding time, shorter holding time is favorable to
obtaining lower shrinkage.
Fig. 9 shows the curve of the sintering shrinkage at different heating rates. The heating rate is increased from 240 C/h to
540 C/h, and the sintering shrinkage is decreased from 1.12% to
0.28%. It can be seen that a higher heating rate is helpful to get a
lower sintering shrinkage and maintain the integrality of complex
ceramic core.
The novel sintering process was dened as follows: at rst, the
ceramic core green body was heated to 600 C with a heating rate
of 60120 C/h and kept 0.51 h; and then heated to1550 C with a
heating rate of 360540 C/h and kept 4 h; nally cooled to ambient
temperature along with the furnace. By adding magnesium oxide
power and adopting sintering process, the sintering qualied rate
of complex-shaped ceramic cores can reach up to 90%.
Fig. 10 shows the injection moulding process and the gelcasting process for complex-shaped ceramic cores. It takes a long time

Fig. 10. Comparison between the injection moulding process and the gelcasting process.

H. Wu et al. / Journal of Materials Processing Technology 209 (2009) 58865891

(78.5131.5 days) to fabricate complex-shaped ceramic cores by

injection moulding, but a relatively short time (1018.5 days) is
required by gelcasting. The injection moulding process is more suitable for mass production, and the SL-gelcasting is more suitable for
new products development as well as single part and small quantity
production.
4. Conclusions
A SL-gelcasting fabrication process of complex-shaped ceramic
cores for gas turbine blades was successfully developed. The conventional air-drying process was substituted by the freeze-drying
process, and the drying shrinkage was decreased from 2.0% to 0.25%,
which is helpful to maintain the structural integrity of complexshaped ceramic cores. The mineralizer (magnesium oxide power)
was added and the reasonable sintering process was determined,
the sintering shrinkage is below 0.50%.
Compared with the injection moulding process, the SLgelcasting process is more efcient in fabricating complicated
ceramic cores, and it is more suitable for new products development, single piece and low-volume production of complex-shaped
ceramic cores. Future research will include investigation on how to
improve comprehensive properties of alumina-based ceramic cores
(including high-temperature properties and room-temperature
properties).
Acknowledgements
This research work was supported by 973 Program of the Peoples Republic of China (Grant No. 2007CB707704) and Program for
Changjiang Scholars and Innovative Research Team in University
(IRT0646). The authors are grateful for the grants.
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