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Surface & Coatings Technology 190 (2005) 15 24

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Laser-assisted direct manufacturing of functionally graded 3D objects


A. Yakovleva,*, E. Trunovaa, D. Greveya, M. Pilloza, I. Smurovb
a
b

LTm, 12, rue de la Fonderie, 71200 Le Creusot, France


ENISE, 58, rue Jean Parot, 42023 Saint-Etienne, France

Received 29 April 2003; accepted in revised form 8 July 2004


Available online 16 September 2004

Abstract
Composition gradients of different types were produced in three-dimensional (3D) objects by means of a repetitive deposition process to
manufacture functionally graded materials (FGMs). Each layer of about 30-Am thickness is created by coaxial powder injection into the
working zone along with the laser beam through a specially designed nozzle. The influence of two different laser sources, pulse-periodic
Nd:YAG (wavelength 1.06 Am) and quasi-continuous wave CO2 (wavelength 10.6 Am), on the process has been studied. Since the former
source provides better beam quality, the pulse-periodic Nd:YAG laser seems preferable for developing FGM components.
The technique used allows developing predefined composition gradients by an appropriate change of the powder composition during the
layer deposition process. The layered FGM samples were examined by metallography, microhardness measurements and SEM analysis. The
compositional gradient can be smooth or sharp. This process also allows development of periodic multilayered structures.
The SEM analysis showed that the minimal transition zone between two different alloys is only about 70 Am for a given condition. Thus,
development of FGM structures by the above process seems feasible.
D 2004 Elsevier B.V. All rights reserved.
Keywords: Cladding; Multilayer; Cobalt; Chromium alloy; Functionally graded materials (FGM)

1. Introduction
The current activities in free-form manufacturing are
mostly centered around the integration of two recent
developments, namely, rapid prototyping (RP) for the direct
manufacturing of parts with complex three-dimensional
(3D) shapes and synthesis of functionally graded materials
(FGM), [1] with variation of physical or chemical properties, e.g. between the core and surface of a component. The
technology of free-form manufacturing of FGM components
is in great demand for several applications [2]. Integration of
RP and FGM technologies promises to extend the scope and
capability of laser-assisted manufacturing dramatically to
the creation of an object with a desired shape and internal
structure, compositional gradients and protective layer in a
single manufacturing process.
* Corresponding author. ENISE, 58, rue Jean Parot, 42023 SaintEtienne, France. Tel.: +33 477910162, fax: +33 477910178.
E-mail address: iakovlev@enise.fr (A. Yakovlev).
0257-8972/$ - see front matter D 2004 Elsevier B.V. All rights reserved.
doi:10.1016/j.surfcoat.2004.07.070

It is possible to combine both RP with production of


FGMs to surface technologies. In RP the object is created
layer by layer and each new material layer is created on the
surface of the previous one. On the other hand, gradual
development of FGM in bulk often implies the repetitive
deposition of layers with varied composition. The possibility to control the composition of each layer allows the
precise regulation of the nature of the FGM gradient during
a process.
The integration of two processes in one can be provided
with the application of particularly organized coaxial
powder injection into the zone of laser beam action [3,4].
It gives the possibility to deposit the material layer with a
spatial accuracy in the range of tens of microns as well as to
change the material composition during the deposition
process [4]. Development of the process needs certain
factors to be considered, such as mutual dissolution of
components/elements leading to the formation of intermetallic phases between layers, wettability between different
components, difference in gas-dynamics and thermophys-

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A. Yakovlev et al. / Surface & Coatings Technology 190 (2005) 1524

in Table 1. The applied stainless steel powder is produced


by thermal spraying, particles with spherical shape and an
average size of 7 Am. Stellite grade 12 powder was a milled
alloy with irregular shape of particles having an average size
of 50 Am.
The substrate is a rectangular piece of stainless steel
304L with dimensions of 30305 mm with a surface
roughness Ra of 3 Am.

ical constants of applied materials. The coaxial nozzle


design and its dependence on geometry and gas-dynamic
conditions have been discussed in Refs. [5] and [6].
However, experimental studies concerning the application
of coaxial nozzle for producing layered FGM are limited in
number. Furthermore, the influence of the radiation modewavelength, pulsed-periodic or continuous wave (cw) on the
process spatial accuracy has not been studied in detail.
Earlier, an attempt was made to develop 3D objects with
powder injection under the laser beam [7]. However, the
nozzle used in this study was not coaxial nor was the
structure compositionally graded. Similarly, the influence of
pulse width on the characteristics of homogenous multilayer
316L stainless steel structure was investigated without
detailed characterization [8].
In the present work, a series of experiments has been
carried out to fill some of the abovementioned gaps and to
examine the ability of coaxial nozzle to produce layered 3D
objects with material gradient. A number of test models
were made with gradients between stainless steel AISI 316L
and stellite grade 12. Special attention was given to the
production of 3D shapes (test wall) with the highest possible
spatial accuracy for the given conditions.

2.2. Experimental set-up


The experimental set-up consists of the following units: a
laser source, a laser beam delivery system, a powder feeding
system, a coaxial nozzle and a CNC table.

2. Materials and experimental set-up

2.1. Materials
The powders for the development of FGM have to meet
certain requirements. First, the powder materials for
fabrication of FGM have to be compatible with each other.
If the process of layer deposition has a stage where at least
one of the components exists in the liquid phase,
wettability becomes the most definitive factor in the layer
formation process [9,10]. This factor is less important for
the sintering process where only part of the particle turns
into the liquid phase and the sintered area is precisely
defined by the zone of laser radiation. But a sintering
mechanism implies a rather high residual porosity of the
consolidated material.
The second requirement is that powders have to be of the
same granularity and shape for the reasons given below in
Section 3.2.
In the present study, stainless steel 316L (SS 316L) and
stellite 12 powders were chosen for the fabrication of FGM
structures. These materials are of interest due to their mutual
compatibility, mechanical and corrosive/wear-resistant properties. The composition of the applied powders is presented

The laser source. Two different laser sources with 10.6and 1.06-Am wavelengths were used. The first one is the
quasi-cw (pulse frequency 3 kHz) CO2 Rofin Sinar
SCx20 laser with radiofrequency excitation and average
power of up to 300 W and Gaussian intensity
distribution. Optics provides a focal spot diameter of
120 Am. The second laser source is pulsed-periodic
Nd:YAG (HAAS HL 304P) with an average power of up
to 300 W. The laser radiation is delivered to the working
zone by a 400-Am optical fiber. Optics provides a focal
spot diameter of 200 Am.
The powder feeder is bPlazma Technik Twin System 10CQ with two independent feeding channels. The applied
carrying gas as well as the shielding/focusing gas is
argon.
The coaxial nozzle creates a conical powder flow
directed to a substrate coaxially with the laser beam
(Fig. 1) and surrounded with a protective/focusing gas.
It consists of three truncated cones inserted into one
another, with certain gaps between them. A carrying gas
with powder is delivered between the internal and the
middle cones, a shielding gas is delivered between the
middle and the external cones (Fig. 1), thus protecting
the melting pool from oxidation as well as providing
powder flow focusing.
The CNC table is used for the displacement of the
substrate within the zone of laser radiation with a
positioning accuracy of ~1 Am.

2.3. Experimental procedure


The following experimental procedure is shown in Fig. 1:
3D FGM samples are fabricated layer-by-layer with powder
deposition on the moving substrate.

Table 1
Component content of stainless steel 316L and stellite grade 12
Component (wt.%)

Cr

Ni

Mn

Mo

Si

Fe

Co

Stainless steel 316L


Stellite grade 12

0.03
2

17
30

12
3.5

2
b1

2.5
b0.8

1
b1

0.045

0.03

Rem
b5

18.5

4.2

Rem

A. Yakovlev et al. / Surface & Coatings Technology 190 (2005) 1524

Fig. 1. The general scheme of the 3D FGM sample build-up process


applying the coaxial nozzle. The arrow shows the direction of the substrate
movement.

In the reported experiment the FGM objects were


fabricated in the form of a thin wall. In this case the wall
thickness characterizes the process limitation in the geometrical detailing of the produced 3D object. The wall
surface quality is a good approximation of the 3D FGM
sample surface accuracy.
The powder feeder has two independent feeding channels
allowing to deliver two different powder types simultaneously, thus creating binary compound, functionally graded
structures. The compositional gradient is achieved by
changing the powder flow content for each channel during
the deposition process while keeping the total powder
volumetric flow and the FGM growing rate constant.
The powder flow was registered with a high-speed CCD
camera. The powder flow was illuminated by the semiconductor laser source (k=670 nm) with a cylindrical lens
providing expansion of the beam into a line, thus allowing
to highlight the flow vertical cross section. The highest
intensity of scattered light is related to the highest density of
the particle flow (Fig. 2). From the data obtained with the
CCD camera, it was noticed that the powder beam profile is
largely determined by the particles shape and granularity.

17

oxidation film creation. This effect is more important for the


CO2 laser because after the formation of the first oxidation
layer the absorption of laser energy increases sharply for a
radiation with k=10.6 Am (CO2) vs. k=1.06 Am (Nd:YAG).
After a relatively long time of slow heating, the temperature
reaches the threshold value which is close to the temperature
of intense oxidation at the given conditions. As the
absorption coefficient is greater for oxides than for pure
metals, a sharp increase of the absorption coefficient
provides likely conditions for powder overheating, which
in turn intensifies the oxidation process.
On the other hand, the use of CO2 radiation is more
convenient due to better beam quality. The present Nd:YAG
laser with a fiber delivery system provides a Rayleigh zone
size of less than 1 mm, while for CO2 laser it is
approximately 5 mm.
The results obtained by using pulsed Nd:YAG and quasicw CO2 lasers are presented in Figs. 3 and 4. These structures
were built from the 316L stainless steel powder (SS 316L).
Metallographic examination of the samples made from
SS 316L indicates that the layers have a fine cellular
structure with no cracks or other defects. This type of
structure is typical for the primary austenite solidification of
stainless steel.
The mode of radiationpulsed or CWsignificantly
influences the geometry and microstructure of the 3D object.
The strip-like structure in Fig. 4 is caused by the contribution
of the different pulses at the considered cross section.
The sample shown in Figs. 3 and 5 is made with a CO2
laser, with an average power of 90 W, scanning speed of 300
mm/min, and powder feed rate of 7.5 g/min. Layer thickness
is about 50 Am. The sample shown in Figs. 4 and 6 is made
with a Nd:YAG laser with a pulse duration of 0.7 ms, pulse
energy of 0.4 J, average power of 80 W, scanning speed of
300 mm/min and feed rate of 7.5 g/min. The thickness of the
layer deposited for one nozzle pass is about 85 Am; each
layer consists of about five sublayers related to the action of

3. Results and discussion


3.1. Comparison of results obtained with CO2 and Nd:YAG
lasers
The important features of 3D FGM objects are their
geometrical characteristics (accuracy, complexity of the 3D
shape), surface roughness and details resolution.
There are well-known characteristics of CO2 and
Nd:YAG laser radiation which can influence the FGM
properties: the powder cloud widens the laser beam due to
the high reflectivity of metals for CO2 radiation, interparticle reflections and scattering, increase in the melt zone
size. Due to the presence of a small amount of oxygen in the
working zone the reflection coefficient will be significantly
time-dependent because of the threshold-like kinetics of

Fig. 2. The powder jet image obtained by the high-speed CCD camera. The
powder jet is illuminated by the lateral laser source.

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A. Yakovlev et al. / Surface & Coatings Technology 190 (2005) 1524

Fig. 5. The contact zone between substrate and synthesized object, made by
quasi-cw CO2 laser.
Fig. 3. The cross section of the wall made by CO2 laser from stainless steel
316L powder, polished, etched.

a single pulse; sublayer thickness is varied in the range 12


25 Am. As adjacent pulses provide a different contribution
to the deposition for a given point, the maximal sublayer
thickness is related to maximal deposition efficiency when
the laser beam is situated just over the investigated crosssection plane.

Fig. 4. The cross section of the wall made by pulse-periodic Nd:YAG laser
from stainless steel 316L powder, polished, etched.

In Figs. 5 and 6 it is seen that the depth of the melting


pool on the substrate is greater for the pulsed mode due to
higher absorbed peak power density: 105 W/cm2 for k=1.06
Am vs. 3d 104 W/cm2 for k=10.6 Am.
The lateral surface roughness is better in the case of the
pulsed Nd:YAG laser due to the reduced quantity of
partially melted particles. This is caused by more local
thermal gradients and shorter life of the melting pool due to
shorter time of interaction with laser radiation during each
pulse.
By changing the parameters of the defined pulses it is
possible to regulate precisely the 3D FGM built-up process.
With a proper choice of operational parameterspulse
duration, pulse energy, pulse shape and frequency, it is
possible to achieve the desired process conditions (HAZ,

Fig. 6. The contact zone between substrate and synthesized object, made by
pulse-periodic Nd:YAG laser.

A. Yakovlev et al. / Surface & Coatings Technology 190 (2005) 1524

melt zone size, cooling rate, etc.) more precisely than for the
continuous wave mode.
The achieved sample wall thickness is about 200 Am for
CO2 and 300 Am for Nd:YAG lasers. It is approximately 1.5
times larger than the laser spot diameter in the working
zone. The obtained height of the wall is about 12 mm and
the length is 25 mm. These dimensions are limited only by
the CNC movement range and substrate area.
3.2. Critical process parameters
The laser-assisted manufacturing process of 3D FGM
objects depends on a number of variables: particle nature
and granularity, powder feeding rate, duration of particle
interaction with the laser beam, laser power density,
scanning speed, relative positions of laser beam waist,
substrate and nozzle outlet. Let us define the most critical
parameters that have influence on the process quality from
the abovementioned ones.
(1) The relation between scanning velocity, power
density and powder feeding rate determines whether a
deposited layer is smooth and continuous or it is divided
into separate segments. This phenomenon is determined by
the temperature-dependent rheological properties of the melt
(viscosity, surface tension, wettability, etc.) and the amount
of melt produced during laser heating. According to Wu
[11], the most important parameters are powder feeding rate
and specific energy defined as E=P/D bV, where P is the
laser power, D b is the beam diameter and V is the scanning
speed. For our experimental conditions the optimal scanning
speed is 40 mm/s, laser power density is about 105 W/cm2
and powder feeding rate is 1 cm3/min.
(2) The distances between the last layer surface, focal
plane and divergence of the laser beam define the stability of
the deposition rate vs. the distance in the direction of sample
movement (direction of y-axis; Fig. 7). The initial instability
of the deposition rate, which is due to the instability in powder
feeding rate, laser power density or scanning velocity, leads to
initial irregularities at the growing surface. At certain
conditions these irregularities can be increased or smoothen
out by subsequently deposited layers due to a certain kind of

19

natural process bfeedbackQ. If the focal plane is above the


growing surface (see Fig. 7; distance baQ is negative), then it is
irradiated by a divergent laser beam. In this case, any
protuberance in the z-direction will be exposed to a higher
power density than a cavity. As a rule, in the cladding regime
higher power density leads to increased growing rate and,
thus, the difference in height between protuberance and
cavity will be further increased. On the contrary, when the
focal plane is below the growing surface, as shown in Fig. 7,
any protuberance is exposed to a lower laser power density
than a cavity, and the height difference between them tends to
be smoothed. All of the abovementioned applies to the
particle flow as wellin the majority of cases the powder
flow has a conical shape, and powder density is dependent vs.
the distance from the nozzle outlet.
(3) The powder flow density at the sample surface
determines the growing rate of 3D FGM. The density
distribution in the powder flow for a given nozzle can be
seen in Fig. 2. In the image obtained by high-speed CCD
camera, the higher intensity of a diffused light corresponds
to higher powder flow density. A cone can be used to
approximate the shape of the powder flow. Maximum
powder concentration is at a distance of 1 to 4 mm from the
nozzle outlet. Therefore, the powder melting efficiency is
determined by the distance from the nozzle outlet. For
applied nozzle, right after the nozzle outlet powder flow is
convergent, then there is the so-called powder flow bfocal
pointQ or zone where powder density is at a maximum and
after that it is divergent, with powder flow density fading
away. Taking into account the reasons from the previous
paragraph, the preferable position of working zone should
be situated just over the powder stream bfocal pointQ.
(4) The particle shape has to be similar and the powder
size distribution has to be narrow to equalize thermal
conditions during heating (e.g. time required to melt a
particle) and cooling stages. It results in the same Reynolds
number that defines the drag coefficient [12] and therefore
particle trajectory after the nozzle outlet. Also, it defines the
cooling dynamics due to the heat exchange with the carrying
gas; this condition is important for unmelted particles
captured by the melting pool. The optimal particle shape
is the spherical one to provide stable powder feeding.
A short theoretical analysis is carried out to define the
optimal process parameters, e.g. preferable particle granularity and the distance between nozzle and substrate.
The following are the applied assumptions:
1)
2)
3)

Particles have an ideal spherical shape


Thermal conductivity kNNh, where h is the heat transfer
coefficient
Latent heat effect is neglected.
The particle motion is derived from the equation

Fig. 7. Schematic presentation of powder-beam interaction zone and critical


distances. The sample shown is in the transversal direction.

dV
3lCD Re

U  V g
dt
4qp D2p

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A. Yakovlev et al. / Surface & Coatings Technology 190 (2005) 1524

where l is the carrying gas viscosity; C D is the drag


coefficient; q p and D p are the particle density and diameter,
respectively; U and V are the velocity of the carrying gas
and particle, respectively; g is gravity constant; and Re is
Reynolds number expressed as
Re

qDp jV  U j
;
l

where q is the gas density.


The drag coefficient C D of flow, for Reb800 is expressed
as [8]
CD


24
1 0:15Re0:687
Re

The change in particle temperature is described by



dT p
6N uk
3Aq
2
Tg  Tp
Dp qp Cp
2qp Dp Cp
dt

where the Nusselt number, Nu=hD p/k, for spherical particles


moving in a gas stream is expressed as
N u 2 0:6Re0:5 Pr0:33 ;

where Pr is the Prandtl number Pr=l/C pk.


By solving Eqs. (1) and (4) one can obtain the temperature profile of the stream of spherical particles vs. the
distance from the nozzle outlet. The graphical solution
obtained numerically for different particle sizes is shown in
Fig. 8. The particle temperature increases quickly after
entering the zone of laser heating, then drops due to
convection heat loss with the surrounding gas and decrease
in laser power density due to the particle cloud shadowing/
scattering effect.
Fig. 8 represents the solution of Eqs. (1) and (4) for
different particle sizes. For smaller particles the temperature
increases more rapidly after entering the zone of laser beam

action due to their reduced heat capacity. This leads to the


displacement of the temperature maximum to the beginning
of the heating process with a decrease in particle size. At the
same time, the heat loss for smaller particles is more
effective due to higher Reynolds number that represents heat
convection with the surrounding gas, leading to faster
cooling. As a result, there is a distance from the nozzle
where temperature curves for particles of two different sizes
intersect. At this point particles of both sizes have equal
temperatures. The condition of particle temperature equality
is preferable for achieving a stable heat contribution from
different particles during the layer deposition process.
There are always short-time instabilities in the feed rate
of separate components with different particle sizes. If flight
distance is not optimized, the particles of different sizes will
have a difference in temperature up to several hundreds of
degrees when they arrive at the substrate. It will lead to
unstable heat contribution to the melting pool and fluctuations of melting pool temperature. These fluctuations lead to
changes in melting pool dimensions and powder catchment
efficiency, which, in turn, can affect the stability of the
geometry and microstructure of a 3D FGM. It also leads to
additional thermal gradients, intense diffusivity of different
components and residual thermal tensions. For this reason, it
is desirable to obtain equal temperatures for components
with different particle sizes. The above is true for
components with similar thermophysical constants and
which differ only in particle geometry (e.g. steel and
stellite). For the components with a significant difference
in thermophysical parameters (e.g. metals and ceramic), the
analysis is similar.
These data are in good agreement with experimental
results, which show that larger particles create thinner layers
at the same power density if distance bdQ in Fig. 7 is less
than that to point bAQ at the graph in Fig. 8. The solution of
Eqs. (1) and (4) allows also to estimate the distance at which
particles are melted.
The following experimental conditions have been applied
to obtain FGM structures: distance till point bAQ (Fig. 8) is 2
mm for a beam divergence of 0.145 radians, distance bdQ
(Fig. 7) is 3.5 mm, the powder feeding rate is 0.017 g/s,
laser power is 90 W (for CO2 laser), scanning speed is 200
mm/min.
3.3. Production of 3D samples with functional gradients

Fig. 8. The dependence of powder beam temperature profile with particle


diameters 7 Am (1) and 50 Am (2) vs. the distance from nozzle outlet. Gas
velocity is 7 m/s, q=5105 W/cm2.

A number of samples have been produced with smooth


or sharp variations in the material content. The minimal
transition zone thickness between two different materials for
sharp variation characterizes the level of gradient detailing.
All graded structures described below are obtained with
quazi-cw CO2 laser source. The tests with Nd:YAG pulsedperiodic laser are a matter of future trials. To build up a
gradient between two materials, an appropriate change in
process parameters is required to keep growth rate and
geometrical parameters stable. Stellite and SS 316L powders

A. Yakovlev et al. / Surface & Coatings Technology 190 (2005) 1524

have close thermalphysical constants for bulk properties


but different granularity and particle shape. As stellite
particles have larger mean size, more laser power is required
to keep the growth rate constant. For SS 316L powder the
average power is 90 W, scanning speed is 300 mm/min and
feed rate is 7.5 g/min. For stellite powder the average power
of 120 W is chosen; all other terms are the same. During
change from one composition to another the laser parameters were changed according to the material concentration
by assuming a linear relation between values related to pure
material (e.g. 105 W is related to 50/50 blend of stellite and
SS 316L).
The following types of graded materials were realized for
the binary compound: smooth gradients (Figs. 9 and 10),
sharp multilayered gradients (Fig. 11), smooth multilayered
gradients (Fig. 12).
Transition zone thickness between two compositions is
mostly defined by the common melt zone size. To achieve a
sharp transition between components, the lifetime and size
of the melt zone should be minimized by means of process
parameters (e.g. pulsed-periodic radiation).
The melt zone size and built-up layer thickness mostly
determine the minimal thickness of transition zone and thus
the achievable accuracy of compositional gradients. There
are some numerical models for heat transfer in a thin wall
[13], but direct measurement of melt zone size/depth should
be done by an appropriate pyrometer or IR camera
diagnostics. Indirect estimation can be done de facto from
SEM analysis data representing the concentration curves of
characteristic elements along a gradient. The width of
concentration curve slope area (concentration change) can
be related to the common melt zone depth where remixing
of elements from adjacent layers takes place. The transition
layer thickness is affected by the fact that residual amounts
of previously deposited powder composition are present in
the delivery tubes and elements of coaxial nozzle, partially
remixing with new composition. Thus, to achieve a minimal
transition layer thickness, powder delivery system should
also be optimized to provide a bclear switchQ between
different materials.
A cross section of a wall with smooth gradient from
stainless steel to stellite is shown in Fig. 9A. Stellite has a
dendritic microstructure that consists of CoCrW solid
solution. The interdendritic region consists of carbides
(M23C6, M7C3). The grain size is about 13 Am and the
layer thickness is about 50 Am. Transition zone size is about
1 mm, with individual layer thickness being about 100 Am.
It is known [14] that stellite corresponds to a two-phase
material with a relatively soft matrix and the reinforcement
phase consists of carbides and intermetallic compounds (e.g.
Co3W) which enhance the mechanical properties. The
increase in SS 316L concentration reduces the contribution
of the abovementioned factors and leads to a gradual change
in the physicalmechanical properties.
The microhardness profile along the graded wall is
shown in Fig. 9C. Microhardness increases with stellite

21

Fig. 9. Sample with smooth stainless steelstellite gradient structure. (A)


Microstructure. (B) SEM analysisthe distribution of components in the
longitudinal direction: the black curve represents the concentration of Fe
(from steel), the gray curve represents Co (from stellite). (C) Microhardness
distribution: zone A is stainless steel 316L, zone B is stellite grade 12, load
50 g.

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A. Yakovlev et al. / Surface & Coatings Technology 190 (2005) 1524

Fig. 10. The sample with smooth stainless steelstellite-stainless steel gradient structure. (A) Microstructure of polished and etched cross section. (B)
Microhardness distribution: zone A is stainless steel 316L, zone B is stellite grade 12, load 50 g.

concentration. This is substantiated by the SEM analysis


(Fig. 9B). In this case the zone of gradient between
components is about 1 mm.
The sample with a similar type of smooth gradient
(316Lstellite316L) is shown in Fig. 10A. The thickness
of an individual layer is about 50 Am with the transition
zone size being about 700 Am. The correlation between
microhardness and composition is shown in Fig. 10B.
Metallographic observation of the cross section (Fig.
10A) shows that dendrites (or columnar grains) sometimes
penetrate through two or three deposition layers.
The minimum value of the achieved separate gradient
zone on the multilayered structure is shown in Fig. 11A. The
transition layer thickness obtained from SEM analysis (first
rising slope of Fe concentration; Fig. 11B) by the abovementioned method is about 70 Am; one layer thickness is

about 100 Am. The task to minimize a transition zone was


not an objective of the present study; this kind of diffused
layer may be beneficial for component integrity. The sample
is built from a repeated sequence of layers (SS 316Lstellite
12). The microhardness distribution along material gradient
is shown in Fig. 11C. The given type of FGM could be
useful for the improvement of mechanical properties, e.g.
shock resistance [15]. The microhardness is more elevated
near the substrate, which can be explained by more intense
heat evacuation (i.e. cooling rate) into the substrate, which
can be considered as a semi-indefinite matter for the applied
conditions. After deposition of the final (top) layer the
additional laser heating with decreased power was applied
to smooth the surface.
The following structure is built up from a repeated
sequence of three different zones (SS 316Lstellite/SS 316L

A. Yakovlev et al. / Surface & Coatings Technology 190 (2005) 1524

23

structures having adjacent layers with different indicative


(key) elements, e.g. Co for stellite and Fe for SS 316L.
Otherwise (e.g. adjacent layers between two kinds of

Fig. 11. The sample with sharp gradient multilayered structure (stainless
steelstellite). (A) Microstructure of polished and etched cross section. (B)
SEM analysisthe distribution of components in the longitudinal direction:
the black curve represents Fe concentration (from stainless steel), the grey
curve represents Co (from stellite). (C) Microhardness distribution:
minimums are related to stainless steel 316l, maximums to stellite grade
12, load 50 g.

mixture (50/50% vol.)stellite layers) (Fig. 12A). Each zone


consists of three layers with average thickness of 50 Am
each. The transition zone value obtained from SEM analysis
(Fig. 12B) is about 170 Am. This value differs from
bminimal transition zone thicknessQ which can be clearly
estimated by SEM analysis only for sharp gradient

Fig. 12. The sample with smooth gradient multilayered structure [stainless
steelmixture of stainless steel and stellite (50/50% vol.)stellite]. (A)
Microstructure of polished and etched cross section. (B) SEM analysisthe
distribution of components in the longitudinal direction. (C) Microhardness
distribution. Maximum values correspond to stellite grade 12, minimum
values correspond to stainless steel, load 50 g.

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A. Yakovlev et al. / Surface & Coatings Technology 190 (2005) 1524

stainless steels), only the width of the concentration curve


sloping area between two relatively close concentrations for
the given component can be considered as the minimum
transition zone thickness, and such a value is difficult to
determine due to the signal noise inherent to SEM analysis
data.
The layer combination applied in the sample shown in
Fig. 12 allows to reduce interlayer stresses between
materials having significant difference in their properties.
Microhardness profile correlates with SEM analysis data
(Fig. 12B,C). The last two samples (shown in Figs. 11 and
12) which are produced from repetitive layers are suitable
for laser hardening effect evolution estimation. The cooling
rate and hence the microhardness are more enhanced near
the substrate for both structures. For smooth gradient
structures, it is difficult to estimate separately the contribution of gradually changed material composition and cooling
rate into the final microhardness distribution (e.g. growing
concentration of more soft material can be compensated by
higher microhardness due to high cooling rate near the
substrate). The microhardness is increased at the top of a
wall as there is only one final deposited layer with relatively
high cooling rate (see Fig. 12C, for example). Along with
this the last layer always represents a finer grain structure
with cell dimensions for stellite of not more than 1.21.5
Am. It is due to the absence of annealing effect from the next
deposition on top. For the sample shown in Fig. 11AC the
effect of top layer hardening is compensated by additional
laser heating with decreased power (annealing) to smooth
the upper surface.
Only the number of powder feeder channels had limited
the number of components combined with the FGM
gradients in produced models.

4. Conclusions
The ability of coaxial nozzle technique to produce
different gradient types in 3D FGM objects from stainless
steel 316L (A) and stellite grade 12 (B) has been
demonstrated.
By varying the coaxially injected powder composition
from layer to layer, the following typical gradient structures
were obtained:
(a)

Smooth transition between two compositions with


smooth gradient zone in a range of a few millimeters.

(b)

(c)

Multilayered structures with alternating layers of


alloys A and B, with a single gradient zone of about
70 Am.
Structures with three consecutive repetitive layers (A/
50% A+50% B/B) with a period of about 150 Am.

The transition zone thickness is determined by the


process variables and can be varied in a wide range. The
achieved process spatial detailing is about 200 and 300 Am
for CO2 and Nd:YAG lasers, respectively. It is approximately 1.5 times larger than the laser spot diameter. The
achieved bwallQ height is up to 12 mm, the length is up to 30
mm and it is limited only by substrate dimensions and the
CNC table displacement range. Certain process parameters
such as the distance between nozzle and substrate, powder
granularity and scanning speed are optimised with the help
of theoretical calculations.

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