Martin P.M. Handbook of Deposition Technologies for Films and Coatings, Third Edition: Science, Applications and Technology
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Evaporation 241
that of the pure matrix material at room temperature by a factor of 1.5–2 at a strain rate of
1.67 × 10
−3
s
−1
(0.1 min
−1
). At high temperatures, the elongation at fracture exceeds 100%,
i.e. superplasticity is developed.
Laminate composites
Laminate composites are attractive and preferable to fibrous composites because of their
uniform properties in the plane of the sheet. In comparison to mechanical methods of
producing laminate composites, e.g. bonding of sheets or foil, PVD techniques are very suited
to the production of such composites, particularly if each lamella is to be very thin (0.01–1 m
thickness) in order to improve the strength and toughness of the composite.
From theoretical considerations, it may be expected that the mechanical properties of
microlaminate composites would follow an adaptation of the well-known Hall–Petch
relationship [249, 250] (yield strength or hardness = αd
−{1/2}
, where d is a characteristic
microstructural parameter such as grain diameter, subgrain diameter, or lamina thickness).
This correlation will be explored later.
In another approach, Koehler [261] proposed that a laminate structure which is formed of thin
layers of two metals, A and B, where one metal, A, as a high dislocation-line energy and the
other metal, B, has a low dislocation line energy, should exhibit a resistance to plastic
deformation and brittle fracture well in excess of that for homogeneous alloys. If the
dislocation-line energies are so mismatched, the termination of the motion of dislocations in
metal B is energetically favored over dislocation propagation across the layer interface into
metal A. In the case of thick layers, the dislocations generated in either of the layers will pile
up in B at the A–B interface and thereby provide the stress concentrations needed for
premature yield. Therefore, to suppress the generation of new dislocations in the layers, the
thicknesses of A and B must be small. Thus, there is a critical minimum layer thickness
required for the generation of dislocations.
This model does not take into account a high imperfection content in the laminate layers but
assumes that their mechanical properties are similar to bulk annealed materials.
Most of the prior work on microlayer condensates was investigated in condensates produced at
low deposition temperatures [262–270] (T < 0.3 T
m
) thus resulting in a high imperfection
content. Moreover, the deposits were very thin (< 25 m in thickness), which makes it very
difficult to measure the mechanical properties (particularly ductility) and draw good
correlations with theory. The systems investigated were Ge/GaAg, Al/Mg, Be/Al, Al/Cu,
Al/Ag, Ni/Cu, Mg/Cu, and Al/Al
2
O
3
.
Recently, Lehoczky [270] studied the layer thickness dependence of the yield strength of
Al–Cu and Al–Ag laminates of thin specimens prepared by alternate vapor deposition. Below
the critical layer thicknesses required for dislocation generation in the layers, the experimental
242 Chapter 4
results are in good agreement with Koehler’s predictions. For layer thicknesses greater than
those required for dislocation generation, he has extended the theoretical model to include
dislocation pile-up groups.
A very recent investigation by Bunshah et al. [204] used high deposition temperatures
(T
∼
=
0.4–0.45 T
m
) where equilibrium structures are formed, and thick specimens
(200–1000 m thickness) containing a very large number of microlayers were produced such
that mechanical properties could be easily measured on standard test specimens. Fe–Cu and
Ni–Cu microlaminate composites were prepared by sequential deposition from two
evaporation sources. Very marked increases in strength were observed, by as much as a factor
of 10 as compared to the pure metals and a factor of 5 as compared to the solid solution Cu–Ni
alloy of the same composition. The ductility decreased somewhat but was still appreciable (5%
elongation) for the highest strength alloys. The strength and hardness values followed the
Hall–Petch relationship. Superplastic behavior was observed in Fe–Cu microlaminates when
the average grain size of the metal equals the interlammellar spacing (approximately
0.45–0.50 m) at a test temperature of 600
◦
C and a strain rate of 0.005 min
−1
.
High-temperature creep properties of thick Fe/Cu and Ni/Cu microlaminate condensates were
studied at 600
◦
C as a function of layer thickness. Steady-state creep rate has been found to
increase with a decrease in microlayer thickness. Microstructural study of the specimens after
creep tests revealed the disintegration of iron and nickel layers in Fe/Cu and Ni/Cu
condensates, respectively, with the formation of separate inclusions of an oval shape. The
creep rate variation in the microlayer condensates is explained with the help of a structural
model of high-temperature creep.
Refractory compounds
Deposits of refractory compounds, oxides, nitrides, and carbides are very important for
wear-resistant applications in industry. Their structure and properties are strongly dependent
on the deposition process. Their behavior is very different from metals and alloys. It is also
very hard to measure the mechanical properties of ceramics by tensile tests similar to those
used for metals and alloys because of their brittle nature. A very good test to measure the
fracture stress of such brittle coatings is the Hertzian fracture test, which measures the fracture
stress and the surface energy at the fracture surface [271]. Colen and Bunshah [136] used this
test to measure the fracture behavior of Y
2
O
3
deposits of various grain sizes.
Figure 4.66 shows the variation in microhardness with deposition temperature for Al
2
O
3
and
ZrO
2
, from the work of Movchan and Demchishin [123], showing that the behavior of these
oxide deposits is quite different in one respect from that of metals (Figure 4.59). The hardness
falls when the structure changes from tapered crystallites (zone 1) to columnar grains (zone 2),
as with metals. However, unlike metals, the hardness increases markedly as the deposition
temperature rises from 0.3 to 0.5 T
m
. The authors attribute this to a more ‘perfect’ material
Evaporation 243
Figure 4.66: Variation of microhardness with deposition temperature for Al
2
O
3
and ZrO
2
.
produced at the higher deposition temperature due to volume processes of sintering. A similar
hardness curve was obtained for Y
2
O
3
deposits [136].
Figure 4.67, from the work of Raghuram and Bunshah [206], also shows a very marked
increase in microhardness of TiC deposits on going from 0.15 T
m
(500
◦
C) to 0.3 T
m
Figure 4.67: Variation of microhardness with deposition temperature for TiC.
244 Chapter 4
(1000
◦
C). The hardness increases for the oxides and TiC with increasing deposition
temperature. Both sets of results may be explained by the following concept. Since the
strength of ceramics is very adversely effected by growth defects and at the higher deposition
temperature the occurrence of these defects is markedly reduced, the hardness (or strength)
increased very significantly. However, it should be noted that the absolute value of the
hardness of the oxides is much lower than that of the carbides. Thus the possibility of a
different explanation for the ‘similar’ behavior of these materials, i.e. the hardness increase
with the deposition temperature, needs to be investigated.
The hardness data on sputtered TiC and TiN coatings are quite similar to those produced by
evaporation techniques [272].
4.11.2 Magnetic Properties
Magnetic nanoparticles prepared by IGC have attracted a lot of attention because it is a
relatively simple preparation method compared to other synthesis techniques. Various metals,
e.g. Fe and Mn, are reportedly evaporated by IGC [49, 273]. The particle size effect on the
exchange bias field for Fe/Fe oxide core/shell structure nanoparticles prepared by IGC was
investigated by Ceylan et al. [49]. The hysteresis curves for particles with different sizes
recorded at 5 K after cooling in 2 T field are shown in Figure 4.68. The effect on the magnetic
properties such as exchange bias and vertical shift is reported to correlate strongly with
structural disorder at the surface of the nanoparticles.
Figure 4.68: Field cooled hysteresis loops for small and large particles at 5 K.
Evaporation 245
Ceylan et al. further reported that two techniques, namely IGC and laser ablation, can be
combined to prepare core–shell structure by evaporating Ni using IGC particles and in situ
coating of Co using laser ablation [76]. The structural and magnetic analyses of the
Ni/NiO/Co
3
O
4
structure showed that these particles had layered core–shell structure and had
improved magnetic properties, such as increased exchange bias due to increased anisotropy of
NiO via interlayer coupling between the NiO and Co
3
O
4
layers.
Ding et al. reported deposition of Co films on the GaAs(001) surface by using an e-beam
evaporation method. The magnetization of the films was found to decrease with increasing
film thickness. They found that slight degradation of magnetic properties could be attributed to
increasing roughness on the Co surface or the Co/GaAs interface during the Co deposition
[274]. Furthermore, multilayer Co/Au was prepared by e-beam evaporation, with Au layer
thickness ranging 5 to 30
˚
A and Co layer thickness of 10–40
˚
A, with a total thickness of 800
˚
A
[275]. Magnetic properties showed strong dependence of remanent magnetization, saturation
magnetization, and coercivity on Au layer thickness related to the effect of interlayer magnetic
coupling.
Kim et al. reported structural and magnetic properties of bcc Co
1–x
Fe
x
(0.1 < x < 0.4) alloy
films prepared on MgO (001) substrates using e-beam evaporation and pulsed laser ablation
deposition (PLD) methods [276]. They found that for x ≥ 0.3 at high substrate temperature T
s
(500
◦
C), alloy films deposited by e-beam evaporation exhibit a bcc (001) growth, showing the
magnetic anisotropy with easy axis parallel to the MgO (100) crystal axis. In the PLD
technique, the excellent bcc (001) film growth is observed at T
s
= 300
◦
C for x = 0.25, which is
close to the concentration limit of the bcc regime in the equilibrium bulk phase diagram,
whereas the same compound films deposited at high T
s
reveal the mixed phase of fcc (001)
and bcc (001) structures. Also, magnetic hysteresis measurements of the film grown by the
PLD technique exhibit similar results to those of the films deposited by e-beam evaporation
[276].
Preparation of thin films by magnetron sputtering is a popular method. However, it has also
been shown that it is possible to prepare magnetic nanoparticles with sputtering, as discussed
earlier in this chapter (PVD Processes). Qiu et al. reported that the L1
0
phase of FePt
nanoparticles can be controlled by modifying magnetron sputtering [277]. Also,
non-conventional (FeCo)
core
Au
shell
and (FeCo)
core
Ag
shell
nanoparticles can be prepared by
combined sputtering and evaporation technique [278]. (FeCo)
core
Au
shell
nanoparticles prepared
by this technique showed a three-fold increase in saturation magnetization compared to that of
iron oxide and better oxidation resistance than FeCo nanoparticles. Bai et al. used the same
technique to prepare (FeCo)
3
Si–SiO
x
core–shell nanoparticles by natural oxidation after
preparation of particles [279].
246 Chapter 4
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