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Surface Modification of Powder


Stuart Barnes Metallurgy Components With a
Michael J. Nash
Y. K. Kwok
Direct Diode Laser
A 1200 W diode laser was used to modify the surface properties of a fully-sintered ferrous
Warwick Manufacturing Group, PM material. Two modifications were investigated; transformation hardening of selected
School of Engineering, areas and sealing of surface porosity by re-melting. The diode laser was used because the
University of Warwick, Coventry, beam footprint is large (50.5 mm) and the wavelength short (0.94 m). Processed
England samples were examined using metallographic and hardness testing techniques. Results
indicated that hardness comparable to induction hardening could be achieved and re-
melting could be controlled to seal porosity. Further work now needs to be undertaken to
convert this demonstrated potential into a commercial reality. DOI: 10.1115/1.1605111

1 Introduction well-established technique for PM components and surface hard-


ening using induction heating to harden just the surface of com-
The production of components via a powder metallurgy PM
ponents is also widely used 5,6. With induction hardening, the
route is well established and accepted in many industries. Com-
depth of hardening is reduced in PM materials compared to
ponents produced range from ferrous automotive gears 1 to su-
wrought steels as the inductance of PM materials is reduced by
peralloy disc alloys for the aerospace industry 2. Although there
the porosity, although this can be overcome by increasing the
are now several variations on the basic PM process used, e.g., hot
power levels used 5. Lasers have been used in materials process-
isostatic pressing HIP and metal injection molding MIM 3,4,
ing for many years 7,8 and although laser hardening is obviously
the components investigated here were produced by a conven-
not an alternative to through hardening, the use of a laser as a heat
tional press and sinter PM process. As this process is well estab-
source to replace an induction coil does offer potential advantages
lished and comprehensively discussed in the literature 5, only a
such as the ability to heat the required area with increased preci-
brief overview of the basic stages of the process will be presented
sion, thus generating less distortion in the component. Such ad-
here. There are three main stages in the production of PM com-
vantages have been acknowledged for several years specifically
ponents via the conventional route. First, the metallic powder and
related to PM components 9 and are regarded as an established
any additives e.g., lubricants are thoroughly mixed together.
advantage of the laser transformation hardening LTH process,
Second, the required volume of powder is placed in a die set of
which is offered by certain specialist companies on a sub-contract
the required physical dimensions and compacted using a hydraulic
basis 10. However, the work reported to-date on LTH has largely
press, this forms a green compact i.e., possessing limited strength
involved the use of the relatively high power CO2 lasers 1.5
due to mechanical interlocking and cold welding of the powder
kW and above with a defocused beam in order to achieve a spot
with the required physical dimensions but limited mechanical
size e.g., 3 mm 11 that was a large enough diameter to make
strength. Third, the green compact is sintered under a protective
the treatment of engineering components viable. Unfortunately,
atmosphere in order to prevent oxidation or decarburisation at a
although the defocusing of the laser increases the beam footprint
temperature below the melting point of the material, solid phase
on the sample, the Gaussian-like distribution of energy within
diffusion takes place which increases the density and provides the
the beam remains 12while such a distribution is ideal for cut-
component with the mechanical properties required in service.
ting applications, for heat treatment it would be more beneficial to
The PM route is generally regarded as a net-shape manufactur-
have the energy distributed as evenly as possible within the foot-
ing process and many components would be regarded as finished
print. Other workers 13,14 have operated the CO2 laser in the
following the three processing stages discussed above. However,
so-called doughnut mode (TEM* 01) as a means of spreading the
there are instances when additional operations, generally termed
secondary operations, need to be performed prior to the compo- laser power over a larger area.
nents going into service. Examples of such secondary processes High power diode lasers HPDLs are a relatively new devel-
would be coining re-pressing, to improve the dimensional accu- opment in laser technology and hence relatively little work on
racy, machining, to produce features that it is not possible to their use for LTH has been reported. Nevertheless, the work that is
achieve during the compaction stage and HIPing to reduce the available, and an examination of the characteristics of the lasers,
residual porosity. Two other frequently performed secondary op- indicates that they are better suited to LTH than the CO2 laser. For
erations were the subject of the work reported here, hardening, to example, their beam footprint is generally line-shaped and it
increase the strength of the components and sealing of the surface can be variable, Ehlers et al. report the use of HPDL with a spot
size geometry which could be varied from 2.6 mm11 mm to 2.6
porosity to prevent the ingress of liquids.
mm22 mm and in addition, within the line-shaped beam the
Providing the composition of ferrous PM materials is suitable
power distribution was uniform and homogeneous. In relation to
carbon levels capable of producing martensite and adequate alloy
heat treatment, another advantage that the HPDLs have in com-
content to give the required hardenability, heat treatment of these
parison to the CO2 lasers is that their wavelength is shorter 1
materials is possible using the same techniques that are used for
m for the diode laser compared to 10.6 m for the CO2 laser
wrought steels 5. Through hardening of PM components is a
which results in a higher degree of absorption of the laser radia-
tion by the material that is being processed. It was therefore ap-
Contributed by the Materials Division for publication in the JOURNAL OF ENGI-
NEERING MATERIALS AND TECHNOLOGY. Manuscript received by the Materials
parent from the above discussion that the HPDL had the potential
Division January 10, 2003; revision received June 17, 2003. Associate Editor: A. to be used for the LTH of ferrous PM materials in fact ferrous
Pelegri and A. Karlsson. materials in general hence the work reported here was initiated.

372 Vol. 125, OCTOBER 2003 Copyright 2003 by ASME Transactions of the ASME

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Fig. 1 Component selected for laser processing; a 100 mm


diameter ferrous sprocket wheel used in automotive engine ap-
plications. Sprocket teeth are induction hardened.

2 Experimental Procedure
2.1 Materials. The specification of the workpiece material
was alloy steel 70AA 0.450.60 percent C, 0.000.30 percent
Mn, 0.450.65 percent Mo, 1.502.00 percent Ni, which is Fig. 2 Laser processing set-up with the laser head positioned
above the component which is held in a chuck attached to a
equivalent to ASTM grade FL-4605-40. The powder had been
CNC controlled X-Y table
compacted and sintered as part of a normal production batch to
produce the component shown in Fig. 1, i.e., a nominally 100 mm
diameter, 4 mm thick disc with a density in the range 6.907.10
g/cc. The sprocket teeth of this component are normally induction result in the deposition of enough material on the cover glass of
hardened following the sintering operation and the discoloration the laser output lens to absorb laser radiation, and cause it to heat
resulting from the hardening can clearly be seen in this figure. The up and shatter.
components that were used for the laser hardening trials were used
in the as-sintered condition without any surface coating or pre-
treatment prior to processing with the laser. It was never envis- 3 Results and Discussion
aged that laser processing would be a competitor to induction
3.1 Initial Laser Hardening Trials. In order to harden the
hardening for the manufacture of this particular component. It was
surface of the workpiece, the laser must raise the temperature
selected for two main reasons. First, the material from which it
sufficiently to transform the microstructure to austenite into which
was manufactured had been selected in order to provide the hard-
the carbon and other alloying elements will dissolve to form a
enability needed for surface hardening, therefore it is possible to
solid solution. This dictated the selection of processing parameters
harden this material and second, the geometry of this component
that would input enough heat to achieve the required temperature
provided a reasonably large area of the surface which was flat and
in the order of 900C, but will not raise the temperature suffi-
could easily be presented to the laser in a suitable orientation, i.e.,
ciently to cause melting of the surface material. As the workpiece
normal to the beam.
was rotated and moved past the stationary laser beam, at any one
2.2 Experimental Procedure. The general arrangement of time a small volume of workpiece material was rapidly heated due
the laser-processing set-up is shown in Fig. 2. The laser used was to the interaction with the laser beam. Subsequently, as that spe-
a ROFIN-SINAR, 1200 W direct diode laser with a beam foot- cific volume of material moves out of the beam, it was then
print of 50.3 mm and a wavelength of 0.94 m. The laser was cooled down extremely rapidly due to self-quenching as the sur-
calibrated prior to carrying out the trials and all power values rounding material, which had remained close to room tempera-
quoted here represent power levels at the workpiece. No addi- ture, removed the heat from the small zone which had been heated
tional lenses were used and the working distance at focus was 90 by the laser. Such self-quenching has been shown to result in a
mm. The workpiece, Fig. 2, was rotated under the stationary laser very effective quench of the austenitized materials with cooling
such that the laser processed a flat section of the component, rates in the order of 104 106 C/s being reported 15. Such cool-
normal to the beam. For all experiments, a nominal flow of nitro- ing rates have been shown to be sufficiently rapid as to result in
gen gas was directed into the processing zone in order to provide transformation to martensite even in steels with low hardenability
an inert shroud over the material being processed especially im- 16. In addition, the rapid heating, the short time that the material
portant when melting of the surface took place and also to pre- spends at the austenitising temperature and the very rapid quench,
vent any smoke particles that were produced from depositing on results in a small prior austenite grain size and a fine martensitic
the output optics of the laser. Although very little smoke was structure in the final product. The heated material was therefore
produced when processing these materials because the surfaces quenched and hardened as it passed beneath the laser beam. As a
where clean and free from deposits of any kind, previous experi- result a hardened track was produced on the workpiece that was in
ence has indicated that relatively small amounts of smoke can the order of 6 mm wide.

Journal of Engineering Materials and Technology OCTOBER 2003, Vol. 125 373

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Table 1 Parameters for initial laser hardening trials and HAZ


hardness results; laser power was 1000 W and the HV load was
100 g

Speed, Depth of HAZ Maximum


Test track mm/min 550 HV, mm Hardness, HV
1 1000 0.82 691
2 1250 0.84 732
3 1500 0.70 640
4 1750 0.58 752
5 2000 0.36 660
6 2250 0.28 537
7 2500 0.14 645
8 2750 0.14 654
9 3000 0.00 501
10 3250 0.00 368
Fig. 4 Hardness profiles produced at a laser power of 1000 W
and indicated processing speeds. It can be seen that the hard-
ness and hardening depth decrease with increasing process-
In order to determine the optimum parameters required to ing speed and that the induction hardened sample is harder
achieve hardening of the surface and identify the depth of such than all laser hardened samples.
hardening, an initial series of hardened tracks were produced us-
ing the set-up discussed in Section 2.2. The laser power was held
constant at 1000 W and the processing speed varied from 1000 to within the HAZ also decreased progressively with increasing pro-
3250 mm/min, Table 1. cessing speed, the data shown graphically in Fig. 6 indicates that
although there is obviously a trend, the correlation is not as good
3.1.1 Examination of Hardened Tracks. The hardened tracks
as was exhibited between the hardening depth and processing
produced by all trials were transversely sectioned at 90 deg to the
speed presented in Fig. 5.
direction of the track, mounted and polished for metallurgical ex-
From an examination of the hardness profiles presented in Fig.
amination. A macrosection of a typical track produced at 1000 W
4, it can be seen that there were two distinct types of profile
is shown in Fig. 3.
depending on the processing speed used. These two types of hard-
The dimension and hardness of the heat-affected zones HAZs
ness profile have also been observed by other workers who have
were then determined by a combination of optical microscopy/
image analysis and microhardness testing. The criteria used to
determine the depth of hardening was the depth at which the hard-
ness was equal to 550 HV and all microhardness tests were per-
formed with a load of 100 g on the indentor. The results obtained
from this analysis of the heat-affected zones are listed in Table 1
and selected data are presented graphically in Fig. 4. A profile of
the variation of hardness with depth was also produced for an
untreated sample to determine if there was any variation in the
hardness with depth before laser treatment, this profile is also
included in Fig. 4 and indicates that there was no variation in
hardness with increasing depth before laser treatment took place.
Examination of the hardness profiles in Fig. 4 suggested that
there was a progressive decrease in the depth to which the laser
processing had hardened the material as the processing speed was
increased. This relationship is clearly demonstrated in Fig. 5,
which shows the variation of the depth to which hardening to 550
HV has taken place, plotted against the processing speed all the
speeds tested have been included in this graph. Although there is Fig. 5 Variation in hardened depth 550 HV with processing
some indication in Fig. 4 that the maximum hardness achieved speed at 1200 W showing a consistent decrease in depth of
hardening with increasing processing speed

Fig. 6 Variation of maximum surface hardness with process-


Fig. 3 Typical laser processed track produced at 1000 W, sec- ing speed at 1000 W. Hardness is reduced at speeds in excess
tioned at 90 deg to the track, polished and etched in a 2 percent of 3000 mmmin, but below this speed the trend is a less con-
Nital solution sistent than that shown in Fig. 5.

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Fig. 7 Martensitic microstructure within the laser processed


track top, and parent material bottom, etched in 2 percent
Nital

laser hardened ferrous materials 13. First, at the slower process-


ing speeds 1000 to 2250 mm/min the maximum hardness
achieved at the surface was within experimental variation main-
tained with increasing depth for a distance below the surface,
before declining with further increases in depth. This is the profile
which would normally be expected from a surface hardening pro-
cess. Second, at the faster processing speeds used 2500 to 3250
mm/min, the hardness achieved at the surface did not extend
below the surface and there was a decline in the hardness with
increasing distance from the surface. Please note that only se-
lected hardness profiles are included in Fig. 4 in order to maintain
clarity.
A more detailed metallographic examination of the samples in-
dicated that at the slower processing speeds 10002000 mm/min
the microstructure produced by the laser processing was marten-
sitic, Fig. 7, which was consistent with the measured hardness
levels. In the case of the faster processing speeds 22503250
mm/min the observed microstructures contained some martensite
but mixed with increasing amounts of nonmartensitic phases e.g., Fig. 8 SEM images of the surface of a untreated material and
pearlite and ferrite. As the quench rates would have been effec- b a laser processed track produced at 1000 W and 1000 mm
tively the same as the previous samples, the incomplete transfor- min, showing the absence of any melting on the surface; see
mation was due to the incomplete austenitization of the room Figs. 11 and 12 for characteristics of a melted surface.
temperature microstructure as there had not been sufficient inter-
action time with the laser beam to transform the microstructure to
austenite There was no indication of cracks within the HAZs of both in an attempt to increase the hardness levels produced at the
any of the tracks produced. Examination of the porosity levels surface, and at the same time investigate the possibility of melting
within the HAZs indicated that this had remained unchanged the surface of the component.
which, combined with the appearance of the surface on which the Laser processed tracks produced during the second series of
laser impinged, Fig. 8, confirmed that no melting of the material trials were examined using the same techniques as described for
had taken place during the heat treatment. the initial series of trials. Figure 9 shows selected hardness pro-
However, although the data in Fig. 4 indicates that the laser
treatment had succeeded in hardening the material at the surface,
the hardness profile which represents the data obtained from an
induction hardened zone produced on the same component during Table 2 Parameters for the second series of laser hardening
trials and HAZ hardness results; laser power 1200 W and hard-
the normal production process, indicates that the hardness level
ness load 100 g
achieved by induction hardening was significantly higher than that
achieved by laser processing, 740 and 925 HV 100 g respec- Speed, Depth of HAZ Maximum
tively. Since surface hardness is an extremely important factor Test track mm/min 550 HV, mm Hardness, HV
when considering resistance to wear or fatigue 17,18 this is ob-
1 600 0.86 913
viously an important factor when considering the viability of any 2 700 0.84 919
surface hardening process. 3 800 0.63 888
4 900 0.58 925
3.2 Second Series of Laser Processing Trials. Due to the 5 1000 0.50 952
relatively low hardness of the initial trials discussed above, a sec- 6 1100 0.53 894
ond series of trials was performed using the parameters detailed in 7 1200 0.50 913
8 1300 0.51 1032
Table 2. In this instance, the laser power was held constant at the 9 1400 0.50 932
higher value of 1200 W and the processing speed was varied 10 1500 0.48 966
between 600 and 1500 mm/min. These parameters were selected

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Fig. 9 Hardness profiles produced at a laser power of 1200 W


and the indicated processing speeds. Surface hardness of all
profiles is comparable with induction hardening although hard-
ening depth decreases with increasing processing speed.

Fig. 12 SEM images of the surface a laser processed track


files obtained. It is evident from the data presented in Fig. 9 that
produced at 1200 W and 600 mmmin, showing a weld-like
the maximum hardness levels obtained from laser processing were surface resulting from significant melting, top right and an as-
comparable with those obtained from induction hardening, i.e., received PM surface bottom left
888 932 HV 100 g and 881952 HV 100 g respectively. Also,

although difficult to see, as the data is so similar, the hardened


depth exhibited by the laser processing produced at 600 mm/min
was effectively identical in terms of hardened depth to that pro-
duced by the induction hardening process, Fig. 9. Although the
hardened depth varied with processing parameters, the microstruc-
tures observed were similar in all cases, i.e., a martensitic outer
layer which, as indicated by the hardness profiles in Fig. 9, tran-
sitioned into a parent metal microstructure over a very short dis-
tance. As with the previous series of trials, the hardened depth
i.e., the depth at which 550 HV was achieved was found to
decrease with increasing processing speed although the correla-
tion was not as good as with the initial trials, Fig. 10.
3.2.1 Sealing of Surface Porosity. Examination of the laser-
processed tracks in the SEM indicated that at all of the processing
parameters investigated in the second series of trials, some melt-
Fig. 10 Variation in hardened depth 550 HV with processing ing of the surface had taken place. At the higher processing speeds
speed at 1200 W showing a consistent decrease in hardness 10001500 mm/min, the melting was relatively limited and the
depth with increasing processing speed resulting surface appeared very smooth when imaged in the SEM,
Fig. 11. In contrast, at the slower processing speeds 600900
mm/min, the amount of melting was more significant and the
resultant track resembled a welding pass, Fig. 12. There was a
progressive increase in the degree of melting throughout the range
of processing speeds used. The increase in roughness with degree
of melting observed in the SEM was also detected in surface
roughness data. The as-sintered surface had a Ra value of 1.64 m
compared to a value of 1.92 m for the laser processed track
produced at 1500 mm/min. However, the track processed at the
slowest speed of 600 mm/min gave a roughness value of 3.39 m
Ra. It is important that when a component is hardened using any
hardening technique, that the surface roughness of the component
is not detrimentally affected by the hardening process. If it is, then
additional grinding operations are generally required to restore the
surface to an acceptable finish.

4 Conclusions
The large beam footprint of the direct diode laser, combined
with the processing speeds which are possible, make the laser heat
treatment of relatively large areas a much more viable proposition
Fig. 11 SEM images of the surface a laser processed track than with the CO2 or Nd:YAG lasers which have much smaller
produced at 1200 W and 1000 mmmin, showing a smooth sur- beam footprints even with a de-focused beam. The work re-
face resulting from limited melting, bottom right compared to ported here has demonstrated the ability of the direct diode laser
the un-melted, as-received PM surface top left to harden a ferrous PM material grade 70AA, ASTM grade FL-

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4605-40 to a maximum hardness of 952 HV 100 g at the sur- by laser melting would need to be investigated relative to the
face and to produce a hardened depth of 0.90 mm as indicated by service requirements of the component. Both the new surface to-
a hardness of 550 HV. Although such depths of hardening were pography and the implications of having a layer of as-cast mate-
comparable with that produced on the particular component inves- rial on the surface of the component would need to be considered.
tigated by induction hardening, it is recognized that the depths of The work reported here represents the initial stages of an inves-
hardening obtainable by laser hardening were far shallower that tigation into the viability of using the HPDL to surface harden
those which are possible with the induction hardening technique. ferrous PM components. Obviously there is a considerable
If required induction hardening can produce hardened depths in amount of further work that needs to be performed in order to
excess of 10 mm. However, because of the higher power density verify the viability of the technique and convert the concept into a
of the laser, and the ability to very accurately control the area of reliable and robust manufacturing process. However, this work
the workpiece which is exposed to the beam and hence heated, it has demonstrated that the technique has sufficient potential to jus-
is possible to heat treat specific areas of the workpiece much more tify further investigation in order to optimize and industrialize the
precisely than would be possible with induction or flame harden- process.
ing techniques. This may be beneficial from the point of view of
reducing the distortion of the component, which all heat treatment Acknowledgments
operations introduce to a certain extent. The maximum hardness
values produced by the laser were comparable with, in fact The authors would like to thank Neil Timms for his assistance
slightly harder than those produced by induction hardening, 952 with the laser processing trials and Peter Worth and Dr. Rebecca
HV 100 g and 932 HV 100 g respectively. However, it should Stewart for their assistance with the microhardness testing and
also be noted that the maximum hardness depth obtained in the SEM analysis. Dr. Barnes would also like to thank The Royal
present work also resulted in melting of the surface of the com- Academy of Engineering for their financial assistance with the
ponent. Defocusing of the laser beam in order to reduce the power presentation of this paper at the ASME 2002 International Me-
density is being investigated as a method of achieving the same chanical Engineering Congress and Exposition in New Orleans.
depth of hardening but avoiding if not required the melting of
the surface. References
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