Basic Powder Metallurgical Aspects in Selective Metal Powder Sintering

J.-P. Kruth (1). B. Van der Schueren, J. E. Bonse. B. Mcrren,

Faculty of Engineering, Department of Mechanical Engineering. Divisiori PMA, Heverlee, Belgium
Received on January 9,1996

A recent evolution in Rapid Prototyping is the direct production of metal parts. The main bottle necks are part
accuracy and appropriate material properties. This paper describes the approach of selective metal powder
sintering (SMS) where liquid phase sintering actions as the basic binding mechanism between individual
metal particles. The merits and drawbacks of this approach are highlighted from metallographic point of
view. Next, a few material combinations, which have been experimentally verified, will be described from
point of view of performance in the SMS process. Simultaneously, solutions for problems related to this
performance are proposed and discussed.

Kevwords: Rapid Prototyping, Sintering, Laser

1. Introduction (50 to 70%). So, a post-treatment is necessary to in-

Selective Metal Powder Sintering (SMS) is a Material
Accretion Manufacturing technology to produce metallic
parts. The main representative of Material Accretion
Manufacturing is Stereolithography [4], introduced in
1987. Material Accretion Manufacturing can be distin-
guished from Material Removal and Material Forming
techniques [S]in the way they make products: they build
products by creating solid (bound) material where it is
needed, without the use of special tools.
Like most Material Accretion Manufacturing techniques,
SMS produces parts in a layer by layer fashion. This
allows a direct coupling with the CAD-model of the
product in which successive cross sections are cal-
culated. Figure l outlines the fundamentals of the SMS
set-up. The basic material is an unbound metal powder
mixture which is spread as a thin layer on top of a
container by means of a deposition system [lo]. Layer
thickness is in the order of magnitude of 0.4 mm. The
powders are bound together using a focused energy
source. During a feasibility study, an electron beam as
well a Nd:YAG laser have been examined [l 11. Since the
electron beam treatment of the powders showed
important technological limitations, this energy source is
not further investigated. The Selective Metal Powder
Sintering set-up is based on a CW Nd:YAG laser, having
a maximum power of 500 Watt. A deflection system
scans the beam over the powder surface according to the
product’s cross section [12]. By carefully controlling the
energy input, the newly created 2D pattern is linked to the
underlying one. Repeating deposition and pattern
creation gives rise to a three dimensional part, called
green product. This green part has a large degree of
porosity and hence poor mechanical properties. The
reason for this is the initial porosity in the loose powder
crease the product’s density. This process might consist
in a thermal treatment or an impregnation with a liquid
metal.
This paper aims to describe the basic binding mechanism
between adjacent powder particles as it is invoked by the
laser beam. The theory is verified using a few powder
mixtures in the experimental set-up depicted in figure 1.
These experiments show the large number of parameters
determining the process behaviour and the resulting part
quality. But, by setting !he right parameters, a broad
variety of different materials and related mechanical
properties become available.
2. Basic Bindina Mechanism in SMS
To create the two dimensional patterns, an appropriate
binding mechanism must be used for binding adjacent
powder particles to form the green part. Two different
approaches are powder melting and sintering (61.
Melting implies a continuous feed of powders in the melt
pool in order to compensate for shrinkage [3]. This may
require complex powder feed and machine control
systems. As all particles must be molten, the process is
relatively. slow but the resulting parts have a high density,
although containing important residual stresses [7].If no
continuous powder feed is applied, shrinkage in the
powder bed during melting results in trapped pores.
These pores may lead to unpredictable mechanical
properties of the parts, since neither size neither location
of the pores is predictable. Figure 2 shows an example of
a copper powder treated by a Nd:YAG laser. The
micrograph reveals a homogeneous metallographic struc-
ture with pores trapped in the centre of the track.
The second approach to consolidate powders consists in
sintering. Distinction has to be made between solid state

Annals of rhe ClRP Vol. 45/1i’1996 183


Figure 1: Overview of the experimental SMS set-up with
indication of fhe main components
sintering (SSS)and liquid phase sintering (LPS). SSS is
a thermal process that occurs at temperatures T:, %Tn c
T, c Tn where T, is the melt point of the powder material.
The driving force for binding is a physical diffusion of
metal atoms from one particle to another. Since this is a
slow phenomenon it makes out the main drawback of
SSS for SMS. Experiments show that a laser beam -
particle interaction time of less than 1 ms is far too short
to initiate sintering.
Liquid Phase Sintering (LPS) is a much faster sinledden-
sification mechanism [Z]. The basic material here con-
sists of a mixture of two metal powders: a high melting
point metal, called the structural metal, and a low melting
point metal, called the binder. Applying heat to the
system causes the binder to melt and to flow into the
pores formed by the non-molten particles.
The main advantage of LPS is the very fast initial binding.
This binding is based on capillary forces which might be
very high: the reaction speed in this stage is determined
by the kinetics of the solid-melt transformation. This
transformation is orders of magnitudes faster than physi-
cal diffusion [a]. Figure 3 gives a qualitative view of the
amount of sintering reaction as a function of time. This
curve shows three different stages: the rearrangement
(melt and capillary penetration), solution precipitation
(grain growth by migration of atoms of the structural metal
through the melt) and a solid state sintering (final densi-
fication).
The SMS process only invokes the rearrangement me-
chanism. Once the binder metal is molten and spread out
into the solid lattice. the system cools down (because the
moving laser beam no longer feeds energy into the sys-
4 conventional
cor LPS LPS in SMS
' bulk liquid phase
ri~itenngof green SMS pan
.- stage 2 (stages 2 6 1)
sdidificafionof i n h l bindinp
liqud !hat ~ s u l l rm g m n SMS part
phase surlenng
Figure 3: Liquid Phase Sintering shows three stages.
from which the first is invoked during laser treatment in
SMS.
184
Figure 2: Cross section of a melt track realised by scan-
ning a Nd:YAG laser beam over a Cu powder bec. Note
the pores in the centre of the track.
tem) and the situation is frozen. This results in green
parts with enough mechanical strength for further post-
processing. In case a thermal post process is applied,
the product will be heated up again and the densification
will continue following the dotted curve of figure 3.
A general remark concerns the post-treatments, which
require an interconnected porosity in the green part. This
means that the pores are connected by means of micro
channels allowing the evacuation of air to the outside or
the flow of liquid metal to the inside. A complete melt
may shut off these micro channels making the densifi-
cation of remaining porosities impossible (figure 2).
3. ExamDles of Workina Powder Systems
This paragraph gives evidence that Nd:YAG laser beam
initiated LPS is possible, that the extent of the reactions
can be controlled and that conventionally used powder
combinations are also applicable in the SMS process.
These examples also show the broad range of various
parameters that must be appropriately set in order to get
the required binding.
3.1 Fe-Cu Dowder mixture
Fe-Cu is a well-described powder mixture for LPS [2,6]
with attractive mechanical properties: the hard Fe lattice
is dispersed in a ductile Cu matrix. New is the laser
initiation of the binding reaction. Previous studies have
shown that a mixture ratio of 20 to 30 wt% Cu is neces-
sary [l 11. This arises from the relative high reflectivity of
the Cu for laser light compared to Fe, meaning that, if no
Figure 4: Nd:YAG laser initiated LPS in Fe-Cu mixture:
white spots are Fe-particles, gray phase is Cu-binder and
black area's are pores.
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Figure 5: Experimentally determinded relationship between laser parameters (laser power and scan speed) and line width
(I) and layer thickness (r)

special precautions are taken. Fe tends to melt before the binder. At lower scan speeds. the applied heat is trans-
Cu particles do what results in a complete melt. The ferred to powder particles that are not directly irradiated
same study revealed a second constraint to the powder by the laser beam. So, in order to accurately control the
particle size distribution: relative smaller Cu-particles width of the laser tracks, it suffices to select a scan speed
enable a better Cu melt distribution. Both constraints for which no heat transfer occurs in the XY-plane. At
result in following powder mixture: Fe (60-90 pm), 30 wt% these scan speeds, the width is in a limited way de-
Cu (25-40 um). The reaction type occurred during laser pendent on the laser power: if not enough power is
interaction is determined by light microscopy of sections applied, no binding reaction occurs. In the other case, the
along the tracks. Setting the right laser parameters laser power may vary up to 10 % without significant
(combination of laser power and scan speed) results in influence on the line width. Similar tendencies are valid
laser initiated LPS as represented by figure 4. This for the layer thickness, that decreases with increasing
picture reveals spherical Fe-particles distributed in the speed and decreasing power level. However, the
Cu-matrix. but simultaneously a large degree of porosity. dependence on power is more pronounced, meaning that
This means that no densification has taken place. This heat penetration in the Z-direction is several powder
observation has also been verified by density measure- particles thick. It allows to control the layer thickness by
ments, showing a density of 50 to 55 wt%, what varying the laser power for a given scan speed in order to
corresponds to the loose powder density. The green get binding between successive layers. Notice that only
samples are typically brittle. This brittleness arises from ihe measurement points with the lowest energy density
oxides that do exist in the powders or that are formed give rise to pure LPS while the others show a more or
during laser heating. To reduce the degree of oxidation, less significant degree of melt. This melting explains the
an inert atmosphere is applied in the reaction chamber by improved heat penetration in the 2-direction compared to
evacuating the chamber to 1 mbar and tlushing it with Ar- the XY-plane.
gon. This allows the creation of useful green parts with
3.2 Cu-coated Fe oowder
limited mechanical properties. A thermal post treatment
The Fe-Cu powder blend has some important disadvan-
of the green samples results in a consolidation of the
tages. Special care must be taken to avoid the Fe-
metallographic bindings with related improved mechanical
particles to melt, a homogeneous distribution of the Cu
strength. The post treatment consists in heating the
particles in the blend is difficult due to gravitational
samples in ti-atmosphere to 1100°C for 30 minutes. This
segregation and oxidation of Fe worsens capillary action
treatment does not significantly decrease the porosity,
(wetting). The most appropriate way to overcome these
what is reflected by a linear shrinkage of just 1 to 2 %.
problems consists in coating the Fe-particles by Cu. The
Two other sample properties are highlighted: the track
coating has been applied through liquid phase electroless
width, being the width of a single line, and the track thick-
deposition [l]. Figure 6-a shows an etched cross section
ness. Both properties are related to the laser power (&)
of a particle revealing a homogeneous layer of Cu over
and the scan speed ( Y I limited to 120 mm/s by the set-
the Fe-core. Note also some impurities in the interface
up), which define the energy density according to:
between both metals originating from the chemical
process.
This powder givfs rise to a more uniform binding,
where 2.W=0.8 mm is the beam diameter on the powder compared to the blend, what is expected since no
surface. Figure 5 shows the experimentally determined capillary action is necessary for the distribution of Cu-melt
relationships. From these results, it follows that the line (figure 6-b). These samples also show a higher degree of
width decreases with increasing scan speed until a width Fe dispersed into the Cu-matrix what should result in
of 0.6 mm is reached. This corresponds to the zone in improved mechanical properties.
the laser spot where enough energy exists to melt the Cu

185
Figure 6: A wide range of material combinations can be treated by SMS: (a) shows a cross section of a Cu-coated Fe
powder while (b) is a laser sintered sample of this powder. (c) represents a WC-Co smtered sample.
Track width and thickness vary with laser power and scan
speed in the same way as the blend, but the settings are
more critical. If the energy density is to high, heavy
reactions occur by which material is erupted out of the
powder surface and no bindings are formed. These
reactions are caused by sublimation of the impurities in
the interface between coating and core material.
3.3 WC-Co Dowder
A third example is a combination of a ceramic powder
WC (prismatic, 225 pm) and a metal binder (Co. irregular.
30 wt%, 20 um). The high melt point of WC and its
chemical stability make that this material is not affected
by the laser. Figure 6-c shows a light microscopy of a
cross section in a sample. It reveals the nice wetting
action of the Co melt, with just few pores (centre of
photograph): the WC particles are well embedded in the
matrix what gives the samples typical hard-metal
properties. The Co matrix is characterised by a high
degree of oxidation, resulting in brittle samples. A better
control of the reaction atmosphere may overcome this
problem. Once again, this powder blend does perform in
the same way as the Cu-based powder systems with
respect to scan speed and laser power, although the
average energy density is shifted to a higher level.
4. Conclusions
This paper has explained two different approaches to
selectively bind metal powders. In case no continuous
powder feed is applied, sintering is preferred over
melting. Liquid phase sintering is most attractive due to
the fast initial binding realised by capillary action. The
examples, covered by the paper, prove that laser initiation
of LPS is feasible, and that a broad range of material
combinations is possible. However, special care must be
paid to the correct blending of the powder systems and
to the problems of laser-powder interaction and oxidation
during heating. Coating of the structural powders with the
binder material is proposed to overcome these problems.
A successful example of Cu-coated Fe-powder is
proposed. Also other powder combinations like WC-Co
prove to be usefull in the SMS process. Finally, two
parameters appear to allow dimensional control of the
tracks: scan speed determines the width of the tracks,
while laser power determines the thickness of the tracks
for a given scan speed.
186
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