Documenti di Didattica
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doi: 10.2298/SOS0802185Z
UDK 662.785:621.798.28
Abstract:
In this article the PIM (Powder Injection Moulding) technology is described in brief.
After that the benefits and advantages were analyzed and summarized. Ceramic injection
moulding (CIM) process was analyzed in more detail: CIM- alumina, CIM-zirconia and CIM
ferrites as the most common technical ceramics in CIM ceramic parts production, medical
applications and accessories in chemical laboratories, and cores in electronic inductive
components. After that our results for CIM barium hexaferrite and piezo ceramics (barium
titanate) are given. The main powder characteristics, the shrinkage and density and the main
electrical characteristics of the sintered samples were compared for the isostatically pressed
PM (powder metallurgy) and CIM formed samples. SEM fractographs of CIM and PM
samples are given for CIM green parts, debinded (white) parts and sintered parts, and PM
green parts and sintered parts. The results obtained were compared to literature data before
they were applied in ceramic components production.
Keywords: Powder injection moulding (PIM) technology, Metal injection moulding (MIM),
Ceramic injection moulding (CIM), Powder granulation, Feedstock, Debinding, Sintering.
1. Introduction
PIM (powder injection moulding) is a net-shaping process, which enables the
production of parts of complex shapes in highly automatised production processes. PIM
allows the fabrication of unique geometric structures that are difficult to produce with other
metal-working technologies. PIM combines the techniques of plastic injection moulding and
powder metallurgy, including sintering. The main process consists of four steps: such as
feedstock preparation, injection moulding (green samples forming), debinding (binder
removing) procedure and the sintering process.
PIM is a metal and ceramic shaping procedure, using a feedstock of composite
granulate. The feedstock is prepared by mixing metal or ceramic powders with plastificators
such as wax, thermoplastics, silicone, agar-agar etc. Melted plastificators enable the powder
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to be injection moulded in the prepared casting tool (green parts). The green parts are then
debinded thermally or by a solvent and finally sintered.
In this work, important factors for PIM applications such as type of material, particle
size, size and sample geometry, and tool casting complexity are discussed. Additional
attention was paid to the sintering of PIM samples: linear shrinkage, weight loss, density,
microcracks and microstructure development. Differences between uni-axial die compacted
and PIM shaped samples in the sintering regime were also analysed.
Examples from literature and practice are given for metal and ceramic powders used
for new PIM shapes. Based on the introduced data, PIM application and its evolution is
analyzed through the introduction of new materials and geometries suitable for technical parts
like electronic components and ceramic sensors.
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in technical ceramic products, electronic components, and medical products. CIM alumina
and zirconia exhibit properties close to the pressed and sintered samples [1,2,3] (see Tab. I).
Calcined alumina powder was selected for the investigation with purity >99.7 %, green
density 3.97 g/cm2 and median particle size <2 m. (chemical analysis [%] Al2O3 99.7,
Na2O 0.05, SiO2 0.05, Fe2O3 0.02, CaO 0.02, loss on ignition 0.01).
Tab. I. CIM densities and surface qualities after sintering, d50 denotes the median particle size
Ceramics
Al2O3
ZrO2
d50 [m]
0.4-0.6
0.2-0.4
Density [g/cm3]
3.85
6.05
Density [% TD]
96.7
99.2
Rmax [m]
3
2
Fig. 1. Microgears of alumina sintered at 1600 C (left) and zirconia sintered at 1350 C
(right).
Fig. 2. CIM alumina products for chemical and medical applications [34].
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Grain size
[m]
5.83
4.80
7.71
4.20
4.50
4.33
n.a.
Rel. density
[% TD]
89.2
87.1
90.4
90.1
85.1
Initial relative
permeability
1518
1305
1238
1360
1463
1463
922.5
922.5
717.7
1609
1456
733.4
716.3
Loss factor
[10-6]
13.21
13.9
17.43 11.71
23.52 21.60
24.15 23.33
37.18
9.0
9.18
50.94 42.06
Tsint [C]/1h
Br [mT]
Hc [kA/m]
BH [kJ/m3]
B
1220
398
290
2.88
1240
402
260
2.61
1260
405
250
2.53
1280
410
230
2.35
1300
399
120
1.19
CIM hard ferrite anisotropy was obtained under a magnetic field of 632 kA/m [15].
The results obtained for magnetocrystalline grain orientation are given in Fig. 3. Anisotropy is
also investigated for injection moulded and pressed polymer bonded magnets: magnetic and
structural properties of Ba M-type ferrite composite powders [16], optimization of ceramic
magnets anisotrope processing [17], of SiO2 and CaO additions on the microstructure and
magnetic properties of sintered Sr-hexaferrite [18], orientation of c-axis of Sr-ferrite particles
in rubber magnets [19]. CIM soft and hard ferrite products (magnetic cores) for different
applications are given in Fig. 4.
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Fig. 4. CIM soft ferrite bobbin cores (left) and hard ferrite magnets (right) [20].
[32, 33].
Tab. IV. Physical characteristics of PZT-BLT piezo ceramics sintered at 1150 C
Composition
PZT
0.9PZT-0.1BLT
0.7PZT-0.3BLT
0.5PZT-0.5BLT
0.3PZT-0.7BLT
0.1PZT-0.9BLT
BLT
Density [g/cm3]
7.61
7.68
7.53
7.37
7.49
7.56
7.44
Grain size
[m]
9.91
2.23
2.20
1.42
2.21
2.23
2.44
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Tab. V. Physical characteristics of PZT-BT piezo ceramics with optimised processing
condition
Composition
Tsint [C]
PZT
0.9PZT-0.1BT
0.7PZT-0.3BT
0.5PZT-0.5BT
0.3PZT-0.7BT
0.1PZT-0.9BT
BT
1100
1200
1200
1250
1250
1300
1350
Density
[% TD]
96.1
96.8
97.0
94.4
86.1
86.0
95.9
Grain size
[m]
2.36
2.86
1.97
3.87
3.71
5.72
2.42
Hence the piezo devices are produced by classical procedures such as tape casting,
isostatic pressing of powder; polymer bonded types and very rarely by PIM technology [32].
The ratio of PZT-binder for the feedstock was 74:26 %vol. Polymers used for binder aimed for
the injection of PZT ceramics are very common: paraffin-wax 65 %, (ethylene vinyl acetate,
polyvinyl alcohol) 35 %. PIM green samples of PZT were thermally debinded and sintered
from 950-1250 C, depending on chemical composition. The green PZT micro components
and morphologies of PZT powders are given in Fig. V. The initial PZT powder was
submicronic. Investigation of the influence of thermal treatment on the morphologies,
dielectric and ferroelectric properties of PZT-based ceramics is continued [34].
(a)
(b)
(c)
Fig. 5 Green PZT micro components (a), depth of green PZT micro component (b) and
micrograph of PZT powder particles (c).
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shown in picture (f). The main properties of sintered PIM and PM samples are given in tab. 6
as follows.
5m
5m
(a)
5m
(b)
(c)
S
N
S
5m
Ferrite core
(d)
(e)
(f)
Fig. 6. SEM fractographs of CIM and PM BF samples magnified 5000: CIM green part (a),
CIM debinded white part (b), sintered part (c), sintered PM (d), ferrite gears shaped by CIM
BF (e), lateral 12 pole magnetization (f).
Material
MIM BF
MIM BF
PM BF
PM BF
Particle size
[m]
dB 95 1.6
dB 95 1.6
dB 95 1.6
dB 95 1.6
Injection
pressure
(MIM)
Pressure (PM)
[MPa]
80
120
200
400
Tsint
[C/2h]
Density
[g/cm3]
Shrinkage
[%]
Remanent
induction
Br
[mT]
Coercive
force
Hc
[kA/m]
1250
1250
1250
1250
5.01
5.05
5.05
5.11
17
17
16.5
16.5
195
195
205
205
94.5
95.5
84.5
86.5
CIM Ba hexaferrite (isotropic) results (SEM Fig. 6 and Tab. VI) are quite close to the
best results of known hard ferrite producers [35, 36]. Our PIM and PM samples (Tab. VI) do
not differ much in density (5.05 vs. 5.11 g/cm3, respectively), and they have similar magnetic
properties. We have not yet produced PIM anisotropic samples (PIM shaping in applied
magnetic field) to compare the results with anisotropic results given in Tab. 3, which is to be
done in the near future.
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particles can be seen very clearly as shown in fig. 7 (b). The sintered microstructure of PIM
samples is achieved by sintering at 1260 C/2h in air. The microstructure of pressed PM green
PZT piezo ceramic samples made of the same powder at round 3-4 times higher pressure
(200-400 MPa) is shown in fig. 7 (d). The fracture surface of sintered PM PZT piezo ceramic
samples achieved at the same sintering profile as for PIM samples is shown in fig. 7 (e). A
small resonant tube with a 0.3 mm thick wall, our second PIM product made of PZT piezo
ceramic, is shown in fig. 7 (f). The main properties of sintered PIM and PM samples are given
in tab. VII as follows.
5m
5m
(a)
5m
(b)
5m
(c)
5m
(d)
(e)
(f)
Fig. 7 SEM fractographs of CIM and PM PZT samples magnified 5000: CIM green part (a),
CIM debinded white part (b), sintered part (c), green PM part (d), sintered PM part (e), piezo
tube resonator shaped by CIM (f).
Material
MIM
PZT
MIM
PZT
PM PZT
PM PZT
Particle
size
[m]
Injection
pressure (MIM)
Pressure (PM)
[MPa]
Tsint
[C/2h]
Density
[g/cm3]
Shrinkage
[%]
dB 50 4
80
1260
7.54
17
Piezoelectric
charge
constants
d33
[pC/N]
532
dB 50 4
120
1260
7.54
17
530
dB 50 4
dB 50 4
200
400
1260
1260
7.41
7.41
16.5
16.2
505
502
The CIM PZT results (SEM in Fig. 7, Tab. VII) are very close to the PZT data given
in Fig. 5 and Tab. IV and available literature data, [32, 33]. The PIM and PM density results
(Tab. VII) are quite close, implying small differences in piezo electric properties as well. Our
main product, micro resonator tube made of PZT ceramics and shaped by -PIM, emits
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acoustic signals in the frequency range of the human ear. The piezo properties attained are
comparable to those given in the literature [21, 28,34]. Our experiments are continuing.
4. Conclusion
Initially, our interest in PIM was to develop some metallic mechanical parts with high
complexity for industrial applications such as micro gears, heat sinks, fly wheel, lock part
cutting tool mechanical parts through using the MIM procedure. Later, experiments were
started with ceramics and then sensor materials: ferrites and PZT ceramics using the CIM
procedure. It was a difficult task to control the functional properties of ceramics by
controlling micro-structural development.
Comparison between PIM and PM (powder metallurgy) samples is a common method
in research of materials, which the authors have also applied in their experiments. The values
to be compared are usually particle average grain size, density and porosity, shrinkage,
hardness, brittleness and the main functional properties of the materials.
Previous results for PM technology was fundamental, thus CIM samples were
followed by PM samples compacted from powder (dry pressed). Two optimisations in
pressures and sintering temperatures were done in parallel to ensure simultaneous analysis of
both (PM and PIM) optimum to achieve the optimum mechanical and electrical, thermal,
magnetic and piezo properties. In all PIM experiments the feedstock was prepared using a
solvent binder system (wax, thermoplast and additives).
CIM samples have the same starting powder particle size (1.6 and 4 m on average
for Ba hexaferrite and PZT piezo ceramics) as such manufactured by PM but differ in
pressure applied: PM pressures are also several times higher. It is well known that pressing
(compacting) gives the first significant contacts between particles, which enhances
subsequent sintering; nevertheless, the PIM route yields excellent results even without this
compacting step.
Of course, direct comparison of products obtained by PIM and PM press-and-sinter
techniques, respectively, is difficult, due to the strong effect of the manufacturing process on
the final properties, but in any case it can be concluded that both for metallic and ceramic
materials, powder injection moulding is attractive for combining complex 3D geometries with
excellent material properties.
5. References
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