Int. J. Appl. Ceram. Technol.

, 5 [3] 243–248 (2008)

DOI:10.1111/j.1744-7402.2008.02226.x

Ceramic Product Development and Commercialization

Low-Pressure Injection Molding of Ceramic Springs

Israel Krindges and Raquel Andreola
Universidade de Caxias do Sul, 95070-560 Caxias do Sul, RS, Brazil

Cláudio A. Perottoni and Janete E. Zorzi*

Universidade de Caxias do Sul, 95070-560 Caxias do Sul, RS, Brazil
Instituto de Fı´sica, Universidade Federal do Rio Grande do Sul, 91501-970 Porto Alegre, RS, Brazil

Injection molding has important advantages over other methods for the production of advanced ceramic parts with
complex shapes. In this work, low-pressure injection molding was used to produce helical ceramic springs using two different
kinds of molds. The ceramic powders used were submicrometer-sized alumina and partially stabilized zirconia. Sintered
alumina and zirconia springs were obtained free of defects, with densities from 96% to 99% of the theoretical value. In
preliminary mechanical tests, these ceramic springs supported axial deformations up to 10% before failure.

Introduction compared with high-pressure injection molding.7,8 In

There has been a growing interest in recent years in
the fabrication of ceramic springs targeted for applica-
tions that demand resistance to oxidative damage or cor-
rosion in harsh environments at room as well as at high
temperatures.1–5 Ceramic springs and windings have
been prepared by machining cylindrical compacts or by
extrusion of sol-derived pastes or ceramic–polymeric mix-
tures.1–6 While the first process is flexible, but expensive,
the latter suffers from difficulties in extracting polymer-
based binders while keeping the spring’s shape unaltered.
Low-pressure injection molding (LPIM) of ceramic
parts has been shown to be well suited for complex
ceramic parts production and has many advantages
This work was partially supported by CNPq and FAPERGS (Brazil).
*jezorzi@ucs.br
r 2008 The American Ceramic Society
fact, LPIM involves a significantly lower manufacturing
cost for dies and less die wears (due to lower molding
pressures and temperatures) and less expensive injection
equipment. These advantages make this forming meth-
od interesting for near-net-shape forming of complex
parts in the range of 100–10,000 units.7,8 However,
lower injection pressures are only made possible by the
use of a relatively large proportion of low-viscosity bind-
ers in the injection mixture. Hence, LPIM usage has
been limited mainly by the difficulties associated with
the process of binder removal. The difficulties encoun-
tered during binder removal are even greater when the
parts have large cross-section and are prepared with
submicrometer-sized ceramic powder.7,8
The ceramic powder plus binder mixture used for
LPIM should be optimized for high fluidity while keep-
ing the ceramic content as high as possible. For the suc-
cessful production of ceramic parts by LPIM, it is thus
244 International Journal of Applied Ceramic Technology—Krindges, et al. Vol. 5, No. 3, 2008

necessary to develop a suitable binder formulation. This For the production of zirconia springs, a home-
is a difficult task, especially for fine particles, as it involves made injection machine was built (maximum load of
a large number of variables related to physical and chemical 300 g) and used to mix and inject the powder/binder
properties of binder components, and the interaction mixture. In the zirconia/binder mixture, the binder
between them and with the powder surface.7,8 content was increased to 15 wt% to improve powder
In this work, we present a procedure for the dispersion in the mixture.
production of ceramic springs by LPIM. Two methods
of molding were tested. Ceramic parts were first produced
by injection into a helical copper coil. Green ceramic Copper Coil
parts were recovered after the removal of copper walls. To obtain ceramic springs with a minimum man-
The second strategy for molding of ceramic springs ufacturing cost, a copper tube was first used as a mold
made use of a brass mold. In both cases our intention (Fig. 1A). The copper helical coil was rolled manually,
was to develop a simple and low-cost method to mold making this procedure cheap and simple to be imple-
helical springs with good reproducibility. The methods mented. The process, however, has the inconvenience
proposed here are well suited for the production
of high-temperature advanced ceramic springs, heating
elements, and ceramic electrical and mechanical devices.
The quality of the sintered ceramic parts was assessed by
density and Vickers hardness measurements. Stress–
strain curves for the ceramic springs were obtained
from compression tests.

Experimental Procedure

Raw Materials and Powder/Binder Mixtures

Commercially available Al2O3 (alumina) powder

used in this work was submicrometer-sized alumina
A-1000SG (Alcoa, Leetsdale, PA), which was used as-
received. According to the supplier’s data, the powder’s
surface area is 9 m2/g, with 99.8% purity (0.04% MgO,
0.03% SiO2, 0.02% Fe2O3, 0.07% Na2O, and 0.02%
CaO) and an average particle size of 0.4 mm.
The commercially available zirconia (ZrO2) used
was TZ-3YS (Tosoh, Tokyo, Japan). According to the
supplier’s data, the composition is 94.8% zirconia,
5.16% Y2O3 (3 mol%), 0.005% alumina, 0.005%
SiO2, 0.004% Fe2O3, and 0.003% Na2O. The densi-
ty is 6.05 g/cm3, the powder’s surface area is 772 m2/g,
and the average particle size is 0.59 mm.
The mixture for injection molding of alumina parts
was made in an LPIM machine (Peltsman MIGL-33,
Minneapolis, MN). The mixture of alumina and bind-
ers for injection was prepared directly in the LPIM ma-
chine, with 86 wt% of alumina and 14 wt% of wax-
based binder (55 vol%). Binder composition was the
same as that used in previous works.7,8 To guarantee Fig. 1. (A) Copper coil and (B) brass mold coated with a green
good homogeneity, the mixture was mixed for 20 h at polytetrafluoroethylene film used for the low-pressure injection
901C before injection. molding of ceramic springs.
www.ceramics.org/ACT LPIM of Ceramic Springs
that the green ceramic parts are recovered only after the
chemical or electrochemical removal of the copper walls.
The alumina-based mixture was injected into the
copper helical coils using a metallic syringe. The alumina
powder/binder mixture prepared in the Peltsman LPIM
machine was hot pressed in a piston-cylinder device to
form cylinders with 22 mm diameter and 40 mm height.
These cylinders were thus fed in the metallic syringe used
to inject the mixture into the copper coil. Both the syringe
and the copper coil mold were heated to B1201C before
injection. Removal of the copper wall was accomplished
by immersion of the copper coils into a nitric acid solution
(50 vol%) or by electrolysis (I 5 140–240 mA, V 5 15–
25 V) in a CuSO4 solution. It takes a few hours to com-
pletely remove the copper wall. During the entire process
of copper removal it is necessary to keep the temperature
below 301C to avoid any flow of the injected mixture.
Brass Mold
The second strategy for molding of ceramic springs
made use of a brass mold lined with a fine polytetra-
fluoroethylene (PTFE) film (Fig. 1B). This antiadherent
film makes mold lubrication unnecessary. The brass mold
was made multipart to simplify the mechanical extraction
of the green ceramic spring after injection.
The alumina mixture was injected into the brass
mold at 901C and 400 kPa of pressure, keeping the
pressure applied for 12 s, using the MIGL-33 LPIM
machine. Pressure, temperature, and duration of the
injection process were varied in order to obtain green
ceramic parts free of defects. Higher injection tempera-
tures promote the formation of small internal bubbles,
whereas higher pressures lead to superficial defects.
After we have successfully produced alumina
springs free of defects, the same brass mold was used
to make zirconia springs. However, given the high cost
of zirconia powder, the ceramic/binder mixture and
injection were made with the aid of a little homemade
injection machine. In this process, temperature and
pressure could not be controlled as accurately as with
the Peltsman LPIM machine. After thorough mixing,
the zirconia powder/binder mixture, heated to 901C,
was mechanically pressed by a piston and injected into
the brass mold previously heated in an oven.
Debinding, Sintering, and Mechanical Tests
The green ceramic parts were subjected to debinding
immersed into alumina powder (A-1000SG), up to a
245
temperature of 2501C (wicking).7,8 After this step, the
parts were fired in air to 10001C, and finally sintered at
16001C/2 h (alumina) and 15001C/2 h (zirconia).
The density of the sintered ceramic parts was mea-
sured by the Archimedes method. Vickers hardness was
measured for loads of 500 and 1000 g. Compression tests
were performed in a mechanical testing machine (EMIC
DL3000, Parana, Brazil) in order to evaluate the spring’s
constant and maximum load and deformation before
failure. Only ceramic springs produced with the brass
mold were used for the compression tests.
Results and Discussion
Molding and Sintering
Alumina powder was used in most of the
experiments. The copper tubular mold had limited
performance as the springs molded with it suffered
from nonuniform spacing between the spring’s turns,
due to difficulties in the manual rolling up of the copper
coil (Fig. 2). Besides that, the rolling-up process has
the drawback of making the spring wire’s cross section
ellipsoidal rather than circular. This distortion, how-
ever, becomes less important as the coil diameter is
made larger. Further improvement in the manufacture
of the copper coil should lead to better molded parts.
The multipart brass mold coated with PTFE improved
the ceramic spring molding process, making it possible
to produce ceramic springs in greater quantities with
good reproducibility.
In the sintering stage, the ceramic springs were
internally supported by an alumina cylinder in order to
Fig. 2. Alumina spring molded in a copper coil.
246 International Journal of Applied Ceramic Technology—Krindges, et al. Vol. 5, No. 3, 2008

Fig. 3. Ceramic springs internally supported by an alumina

cylinder for the sintering stage.

avoid major distortions (Fig. 3). This support allowed

the parts to shrink while sintering without being
mechanically constrained. No cracks were observed
after debinding and sintering, and ceramic springs
with well-defined shapes were obtained, as shown in
Fig. 4.
Table I gives some typical dimensions for the
ceramic springs produced with the copper coil and the
brass mold. The outer diameter and wire diameter of
the green ceramics molded with the brass mold were 32
and 5 mm, respectively. After sintering, the outer diam-
eter and wire diameter for alumina and zirconia springs
were reduced by about 19% and 25%, respectively. The
greater uncertainty in the wire diameter of the ceramic
springs produced with the copper coil mold results from
the ellipsoidal cross section induced by the rolling-up
process. The change in wire spacing after sintering
depends on the way in which the spring is supported
inside the high-temperature furnace. The deviation in
coil spacing after sintering (expressed as one standard Fig. 4. (A) Alumina and (B) zirconia sintered springs injected in
deviation) was about 15% and 10% for ceramic springs the brass mold.
molded with the copper coil and the brass mold,
where D is the mean diameter of the spring, d is the
respectively.
wire diameter, G is the shear modulus of the spring’s
Table II presents density and Vickers hardness
material, and Na is the number of active turns.11
results obtained for the alumina and zirconia springs,
both in good agreement with the literature.9,10 Table I. Typical Dimensions (and Standard
Deviation) of the Ceramic Springs Produced with the
Mechanical Tests Copper Coil Mold and the PTFE-Coated Brass Mold

The spring constant (K) of a spring depends on its Copper coil mold Brass mold
dimensions and material properties. For a typical helical Composition D o (mm)
 d (mm) D o (mm) d (mm)
spring, such as that represented in Fig. 5,
Alumina 25.570.5 2.570.5 26.570.3 4.070.1
Gd 4 Zirconia 24.070.5 2.070.5 24.070.3 3.870.1
K ¼ ; ð1Þ
8Na D3 D , spring outer diameter; d, wire diameter; PTFE, polytetrafluoroethylene.
o
www.ceramics.org/ACT
Table II. Density and Vickers Hardness of Alumina
and Zirconia Ceramic Springs
Vickers Vickers
hardness hardness
Green Sintered 500 g
density density load
Composition (g/cm3 ) (g/cm 3 ) (kgf/mm 2 ) (kgf/mm 2 )
Alumina 2.6670.01 3.8770.01 1659721 1627715
Zirconia 3.3870.01 6.0170.01 139778 138777
Figure 6 shows some results obtained from com-
pression tests carried out with ceramic parts produced
with the brass mold. In compression tests performed
with alumina springs, the maximum applied load before
failure was 9077 N, and the relative deflection
(erel 5 Dl/l0) was 9.471.0%. The quoted uncertainty
refers to the mean’s standard deviation for a set of
20 measurements. In addition, 10 zirconia springs
were tested and failure occurred for an applied load
of 96710 N and erel 5 1272%. Both alumina and
zirconia springs follow Hooke’s law, with spring con-
stants around 250 and 160 N/mm, respectively, which
conforms to the lower shear modulus of zirconia
in comparison to alumina.12
Fig. 5. Schematics of spring design.
LPIM of Ceramic Springs 247
1000 g
load
Fig. 6. Compressive load versus displacement for two ceramic
helical springs.
Conclusions
Alumina and zirconia helical springs were produced
by LPIM. After sintering, parts molded with sub-
micrometer-sized powders were obtained with high
density and good mechanical properties. Mechanical
failure of alumina and zirconia springs occurred under
loads around 90 N and relative deflections about 10%.
Ceramic parts with good reproducibility were obtained,
particularly with the PTFE-coated brass mold. Further-
more, provided that the binder composition and the
ceramic volume loading in the injection mixture are
correctly chosen, the method should be applicable
to ceramic and metal powders in general. Uniformity
in sample preparation and testing conditions allowed a
better comparison of the effect of the ceramic material
on the spring’s properties. The effect of the microstruc-
ture on the spring’s properties as well as the possible
electronic, mechanical, thermal, and tribological appli-
cations of the helical ceramic springs should be further
investigated.
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