Chapter Six

Results and Discussions

Processing and Characterization of P/M Parts:

Introduction:

The characterization of the Cu- Al2O3 sintered system included examinations of

mechanical properties (compression strength, wear, and microhardness), examination
of microstructure by the scanning electronic microscopy (SEM), the energetic
dispersion spectroscopy (EDS), examination of structural changes using XRD.

soft matrix/hard dispersion nanocomposites.

Image Analysis:

with a mean size.. nm and a standard deviation of . nm; the size distribution
calculated by the image analysis is shown (in Fig).

Structure:

microstructure survey of the sample sintered at 800C for 30 minutes is given, and it is
clearly seen that the structural stabilization process is not completed. The
microstructure is characterized by the formation of closed pores, which is typical of a
medium stage of sintering, and also, in certain areas, by achieving contacts between
certain particles, which is typical of the starting sintering stage. a relatively even
distribution of pores can be seen in the examined samples, which, among other things,
significantly contributes to the reinforcement of the highly conductive copper matrix.
finely dispersed particles and their homogenous distribution in the base metal matrix
cause stabilization of dislocation substructure formed during deformation and the
achievement of significant reinforcing effects by A complex action of different
mechanisms.

......... of sintered samples indicate a change in the lattice parameter on the grain
boundary, where raster and fingerprint variations can be detected. This leads to the
conclusion that, due to the presence of alumina, the eutectic reaction (Cu+Cu 2O) with
Al2O3 occurred and the third, CuxAlyOz phase was formed, which is possible on Cu-Al
contact surfaces from the thermodynamic point of view.. . .. .. the reinforcement of the
copper matric occurs due to the mechanisms: dispersion and reinforcement due to the
dispersion of the fine particles of Al2O3in the matrix, and the reinforcement of grain
boundaries due to the appearance of the third phase.

The shape of particles is irregular, with the presence of individual particles of nodular
shape. The surface morphology is rough. Apart from that, the presence of an
agglomerate with the magnitude of >100nm and of a sponge shape is noticeable.

XRD

The type of bonding reflected by this work of adhesion value at the interface between
the Cu nanoclusters and the Al2O3(0001) is considered to be metallic and not oxidic.

since Cu-O-Al bonds are generally predicted to be stronger than Cu-Al bonds, thus
leading to increased wetting of the Cu overlayer.

the possibility of Cu aluminate (CuAl2O3) formation.

the peaks can be readily indexed to pure copper (JCPDS file No. 04-0836).
The average grain size of the powder is calculated to be around 70 nm according to
half width of the strongest diffraction peak using Debye-Scherrer formula.

The diffraction peaks are broadened due to the small size of the products.

An unidentified peak was also detected. According to previous studies, [Entezarian &
Drew, 1996; Jena et al., 2001, 2004], this peak corresponds to the third phase,
CuxAlyOz, which appears in the structure due to the eutectic reaction of (Cu+Cu 2O)
with Al2O3. The formation of this phase is thermodynamically posible on Cu-Al
contact surfaces. During the eutectic joining of copper and Al2O3, the eutecticum
formed by heating up to the eutectic temperature expands and reacts with Al2O3 also
forming CuxAlyOz, which is compatible with both phases on the intersurface. The
formed third phase influences the nature of the dislocation structure and also the
improvement of the mechanical properties and the creation of a good combination of
mechanical and electrical properties of the sintered systems.

Except for copper and alumina, diffractive fields are not identified, which is typical of
some other phenomena (e.g. appearance of the third phase). The reason for that could
be the common limitations of the technique, i.e. the determined critical value below
which the phases cannot be identified.. . . . . Finally, apart from the stated, the obtained
results of the examinations confirm the crystal nature of copper and dispersed alumina.

This leads to the conclusion that, due to the presence of alumina, the eutectic reaction
(Cu+Cu2O) with Al2O3 occurred and the third, CuxAlyOz phase was formed, which is
possible on Cu-Al contact surfaces from the thermodynamic point of view.

the eutectic reaction occurred and the third, CuxAlyOz phase was formed on the grain
boundary.
SEM, EDS, & Morphology

The shape of particles is irregular, with the presence of individual particles of nodular
shape. The surface morphology is rough. The agglomerates of the size >100nm,
formed by the individual particles of the stated size are also observed. The
agglomerates are of a spongy shape. Since the powders with exceptionally fine
particles are obtained by the previously described procedure, the basic "condition" for
the appearance of agglomerates is fulfilled. Namely, agglomeration of finer particles is
a consequence of their large surface and high surface energy, respectively, and of the
effect of attracting forces acting between them. The creation of attracting strains, the
magnitude of which depends directly on the surface energy of the particles which are
in contact, occurs on contact surfaces due to the atomic connections in the interface.

the obtained results of the examinations confirm the crystal nature of copper and
dispersed alumina.

An estimation of the impurity level was performed by energy disperse spectroscopy

(EDS) analysis with a Si(Bi) X ray detector, connected with the SEM and a multi-
channel analyzer. An EDX-System Oxford Link ISIS with HPGe- Detector and UT-
Window was used for chemical analysis of microscopic volumes for all elements with
atomic number > 4.

In order to determine the distribution of elements in the structure, the surface analysis
of the sample was performed by EDS.

the grain size is anything but monodisperse in actual nanocrystalline samples. The
internal structure is poorly described by a single grain size.

In order to determine the distribution of elements in the structure, the surface analysis
of the sample was performed by EDS.
analysis of the sintered systems reveals the presence of copper crystals of 100 nm in
size.

examination of microstructure by the scanning electronic microscopy (SEM), the

energetic dispersion spectroscopy (EDS).

Sintering

Almost any deviation from pure single-phase material will reduce the tendency for
grain growth. This includes residual pores, impurities and solutes, and second phase
particles, all slowing down grain growth. Pinning by fine particles is, in fact, a very
efficient way of slowing or stopping grain coarsening.

Grain growth can be hindered by a narrow size distribution, and by impurities. . . . .

Almost any deviation from pure single-phase material will reduce the tendency for
grain growth. This includes residual pores, impurities and solutes, and second phase
particles, all slowing down grain growth. Pinning by fine particles is, in fact, a very
efficient way of slowing or stopping grain coarsening.

A retardation of the normal crystallite growth. presumably arises from interface

pinning due to solute impurities, impurity-related second phases, or residual porosity.

A retardation of the normal crystallite growth, presumably arises from interface

pinning due to solute impurities, impurity-related second phases, or residual porosity.

suggest a correlation between the thermal stability and the presence of nanopores.

A promising strategy for the controlled stabilization of nanocrystalline metals, in

addition, for example, to interface pinning by oxide or carbide nanoparticles.
Mechanical Properties

Compression Test

Strength

the reinforcement of the copper matrix occurs due to the mechanisms: reinforcement
due to the dispersion of the fine particles of Al2O3in the matrix, and the reinforcement
of grain boundaries due to the appearance of the third phase.

Wear Test

This study used pin on- disk to assess the resistance of as-sintered nanocomposite
materials.

Archard law states that the wear resistance is directly proportional to the hardness of
the material.

there is/is no simple relationship between hardness and abrasive wear resistance. For
these materials the highest hardness did/ did not correspond to the highest wear
resistance.

From these studies it can be concluded that the high hardness of nanocrystalline
materials is a prerequisite of high abrasive wear resistance.

At 50 N, the wear rate first decreases with increasing filler content up to 12 vol.%, and
then increases as the nanotube content reaches 16 vol.%. This can be attributed to the
high porosity content (4.92%) in the Cu/16 vol.% MWNT nanocomposite. Thus, the
wear rate of copper nanocomposites depends greatly on the microstructure and applied
load under dry sliding conditions.

Ductility

a better correlation was found between ductility and wear resistance.

for equal hardness/grain size, the other important factor is ductility, with lower
ductility giving better abrasive wear resistance.

ductility (>13%) at strength ( MPa) for ( x ) samples of copper with average grain
sizes of several hundred nanometers.

Hardness

These hardness values are equivalent to the compressive failure stress.

Microhardness tests were performed with a 200-g-load Vickers indenter. At least 20

individual hardness measurements were made on each sample. The typical limit of
error on the hardness values was about 0.15 GPa.

Elastic Properties

the presence of extrinsic defectspores and cracks, for examplewas responsible for
the low values of E in nc materials compacted from powders, when compared with
fully dense conventional composites.