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Abstract
Hard and refractory TiC has been deposited on 6061 Al alloy by Laser Surface Engineering LSE.. A composite
coating is obtained with TiC particles of various shapes and sizes embedded in Al alloyTi matrix. The coating is uniform,
continuous and free of cracks. The various reactions occurring during laser processing were thermodynamically analyzed and
related to the experimental observations. Microhardness measurements suggested high hardness values in the coating region
and a strong bonding at the coatingrsubstrate interface. Dry sliding wear tests were performed to measure the wear
resistance and the coefficient of friction of the coating. Wear resistance of the coated surface was found to be high when
compared to the substrate side. The coefficient of friction was found to be 0.64. q 2000 Elsevier Science B.V. All rights
reserved.
Keywords: Laser surface engineering; TiC particles; Wear; Coating; Bonding; Interface
0169-4332r00r$ - see front matter q 2000 Elsevier Science B.V. All rights reserved.
PII: S 0 1 6 9 - 4 3 3 2 9 9 . 0 0 3 6 8 - 2
66 L.R. Katipelli et al.r Applied Surface Science 153 (2000) 6578
material. In such case, Laser Surface Engineering made from commercially available resins used in the
LSE. offers to improve the surface properties of Al paint industry. was spray deposited on the 6061 Al
alloys while keeping the bulk properties more or less substrate. The addition of 10 wt.% Si to the TiC
intact. By means of a high power laser, very high powder was intended to increase the wettability and
temperatures can be reached to melt both the metal fluidity of Al w6x. The average sprayed precursor
substrate and, sometimes, the ceramic particles. This thickness was 150 mm. Sprayed coupons were dried
may promote chemical reaction and wetting between at 708C for 1 h prior to laser processing.
ceramic and metal, and, as a result, may lead to a A 2-kW Rofin Sinar continuous wave Nd:YAG
strongly bonded ceramicmetal interface after reso- laser equipped with a fiber optic beam delivery
lidification w2x. Moreover, LSE involves high cooling system was employed for laser treatment of the
rates 10 3 10 8 Krs. which produce meta-stable sprayed substrates. The optical fiber was 17 m long
phases, leading to the development of a wide variety and 600 mm in diameter. The laser beam was fo-
of microstructures with novel properties that cannot cused at 0.5 mm above the surface of the substrate.
be produced by any conventional processing tech- The lenses within the output-coupling module of
nique w6x. fiber optic were configured to provide a beam of 3.5
Many researchers have studied the effect of ce- mm wide line in spatial distribution onto the sample
ramic coating on Al alloys w711x. However, studies surface. Such configuration provides a rapid process-
on the influence of laser treatment of Al alloys for ing speed and reduces the overlap between the laser
ceramic coating are very limited w2,12,13x. In the passes. There was a 20% overlap between two con-
present study, hard TiC is deposited on Al 6061 secutive laser tracks. The laser beam power and
alloy by LSE technique. traverse speed were maintained constant at 1.8 kW
and 120 cmrmin, respectively. The coated samples
were additionally cooled by mounting them on a
2. Experimental procedure water-cooled copper plate during laser processing.
2.1. Materials
2.3. Characterization
Commercially available TiC powder 99.5% pu-
rity and average powder size - 15 mm. and 6061 Al Phase identification was carried out on a Philips
alloy were used in the present study. The TiC pow- Norelco X-ray diffractometer with CuK a 1.54 A
der was supplied by CERAC Milwaukee, WI. The wavelength. radiation, operating at 40 kV and 20
chemical composition of 6061 Al alloy is given in mA. X-ray diffraction XRD. analysis was per-
Table 1. formed on both the worn and unworn surfaces of the
coating to determine the possible changes in phases
2.2. Coating process as a result of wear tests. Microstructural characteriza-
tion was performed on an ISI super III-A scanning
Plates of 6061 Al alloy with dimensions 12 = 12 electron microscope SEM.. The samples for metal-
= 1 in3 were cleaned using sand blasting. The pow- lography were prepared by sectioning the coated
der precursor made of 90 wt.% TiC q 10 wt.% Si plate perpendicular to the laser tracks. The sectioned
suspended in a 10-wt.% hydroxyl methyl cellulose faces were polished on a Buehler Isomet 2000 cloth
water-based organic binder proprietary formulation to a diamond finish. Kellers reagent was used as the
etchant. Energy dispersive spectroscopy EDS. and
X-ray mapping equipped with SEM were utilized to
Table 1 determine the elemental distribution in a semi-
Chemical composition of 6061 Al alloy in wt.% quantitative manner. Macroscopic observations of
Mg Si Cu Cr Mn Fe Al the cross-section of the coating were also conducted
0.81.2 0.40.8 0.050.4 0.040.35 - 0.15 - 0.7 Bal. under BX60M Olympus microscope. This high-reso-
lution optical microscope was equipped with differ-
L.R. Katipelli et al.r Applied Surface Science 153 (2000) 6578 67
ent modes of light to observe the cross-section in generation of stoichiometric andror non-stoichio-
desired light conditions. Microhardness tests were metric derivations. Primarily, in the system under
performed on a Buehler Isomet microhardness tester investigation, the following reactions are possible.
with a Knoop indentor under a normal load of 200 g The free energy of formation and their temperature
applied for 15 s. Dry sliding wear tests were carried ranges are obtained from various sources w1418x,
out on a Block-on-Disc tribometer to determine both
the weight loss and coefficient of friction with re- Ti q C TiC 1.
spect to time. The speed of the rotating disc was
maintained at 4.4 mrs and a normal load of 4 lb was DG s y182.9 q 0.01T kJrmole 298 - T - 115 K.,
applied to the sample while sliding. These tests were DG s y186.4 q 0.013T kJrmole 1155 - T - 2000
carried out on coated coupons of size 20 = 25 mm2 K. w14x. From the TiC phase diagram, it has been
for a total 20-min duration. Weight loss measure- corroborated that TiC x x F 1. exists as a single
ments were made after successive 2 min. Coefficient homogeneous carbide phase with a wide range of
of friction was also computed simultaneously by an stoichiometry w15x. The reaction is reversible and,
interfaced computer that acquired data in the form of hence, it is possible for Ti and C dissociated from
voltage and current of the motor as a function of TiC to combine with other reacting elements. Ac-
time. cordingly, the following reactions may be consid-
ered:
Si q C SiC 2.
3. Results and discussion DG s y71.258 q 0.0078T kJrmole 0 - T - 1700
K., DG s y120.3 q 0.0368T kJrmole 1700 - T -
3200 K. w16x;
3.1. Thermodynamic predictions
4r3 Al q C 1r3 Al C 4 3 3.
It is essential to study the thermodynamics of the
system to understand the nature of chemical reac- DG s y71.315 q 0.013T kJrmole 0 - T - 900
tions taking place during the coating process. There- K., DG s y91.055 q 0.033T kJrmole 900 - T -
fore, in the present study, attempts are made firstly 3200 K. w16x;
to thermodynamically predict the possible reactions
and, secondly, to verify the existence of these reac-
Ti q 3Al TiAl 3 4.
tion products using analytical techniques such as DG s y52.503 q 0.021T kJrmole 0 - T - 3200
EDS and XRD. Such combined thermodynamic and K. w17,18x;
TiSi
analytical approach provides an insight into the me-
chanical, chemical and thermophysical properties of Ti q 2Si 2 5.
the coated sample. However, it is pointed out that
often the thermodynamic conditions that prevail dur- DG s y134.19 q 0.0067T kJrmole 298.15 - T -
ing laser processing deviate from equilibrium condi- 1700 K., DG s y1.5738 q 1.0063T kJrmole 1700
tions, thereby making equilibrium phase diagram - T - 1813 K. w19x. With the obtained values of free
consideration less applicable and more difficult to energy of formation, a graph of DG vs. T is plotted
predict the process products. Due to the fact that in Fig. 2. From the figure, it is clearly observed that
laser processing is a very complex non-equilibrium TiC is the most stable compound followed by TiSi 2 .
process and also because of the lack of data in the This fact is also evident from the XRD peaks of TiC
open literature on various reaction products during and TiSi 2 shown in Fig. 1.
such non-equilibrium processes, a first approxima- As mentioned earlier, titanium carbide exists as a
tion that generation of products based on equilibrium single homogeneous phase, TiC x with a wide homo-
phase diagrams can be considered. These equilibrium geneity range. The crystal nature of such phase is
products can be considered as sources for further cubic of NaCl type and for TiC of stoichiometric
68 L.R. Katipelli et al.r Applied Surface Science 153 (2000) 6578
composition, the lattice parameter varies between of Al 4 C 3 , Si levels above 8 wt.% are required. In the
4.315 and 4.324 A. Similarly, silicon carbide exists present experiments, though Si in the precursor was
in the form of cubic b-SiC and hexagonal a-SiC. 10 wt.%, it was not sure how much was available as
b-SiC with cubic crystal structure of ZnS type has a free Si in the melt during processing. In view of all
lattice parameter of 4.358 A w20x. The values of these scenarios, it is less likely that Al 4 C 3 will form.
lattice parameters for both TiC and SiC being close, This was further confirmed by XRD analysis Fig.
the X-ray reflection peaks of these phases overlap as 1..
observed in Fig. 1. In addition to reaction 4., TiAl 3 can form via the
Even though thermodynamically Al 4 C 3 is ex- following reaction w7x:
pected to exist up to 29278C Fig. 2. in vacuum, it is
stable up to 12008C and, at 22008C, it sublimes
TiC s . q 3Al s . TiAl s. q C
3 7.
without melting w21x. In addition, the solubility of In the temperature range of 11501800 K, the Gibbs
carbon in aluminum is only 0.020.04 wt.% at energy of formation DG . for this reaction is posi-
130015008C and, at 100011008C, it is practically tive, which indicates that TiAl 3 is unstable for an
zero w21x. Also, the possibility of formation of Al 4 C 3 ideally dilute carbon concentration of 1 wt.%. How-
through carbothermic reduction of SiC exists. Thus, ever, TiAl 3 is stable in the presence of TiC when
Al 4 C 3 may form in the reaction w22x DG becomes negative at concentration of dissolved
4Al q 3SiC Al C q 3Si
4 3 6.
C lower than the 10y5 wt.% w17x. Therefore, TiAl 3
formation can only be expected during processing if
However, the content of SiC and the duration of Ti concentration is very high. Such extremely low
contact between SiC and the molten Al controls the concentration of C may be possible during the pre-
formation of Al 4 C 3 w23x and, for complete stability sent process due to formation of SiC via reaction 2..
L.R. Katipelli et al.r Applied Surface Science 153 (2000) 6578 69
Table 2
Wetting of some refractory carbides by molten metals
Carbide Wetting melt Temperature 8C. Atmosphere Contact angle in degrees Reference
TiC Fe 1550 Hydrogen 39 w24x
Co 1500 Hydrogen 36 w24x
Ni 1450 Hydrogen 17 w24x
Si 1500 Vacuum 32 w14x
Mg 1300 Vacuum 50 w14x
Al 700 Vacuum 118 w14x
WC Fe 1500 Vacuum 0 w24x
Co 1500 Hydrogen 0 w24x
Ni 1500 Vacuum 0 w24x
Si 1500 Hydrogen 0 w14x
Mg Not available Not available Not available Not available
Al 1000 Vacuum 135 w14x
The LMZ has an approximate depth of 300 mm. Fig. c., and d., respectively. Ti-rich zone shows the
4 shows the high magnification micrograph of the presence of TiC particles whereas the coating matrix
interface of LMZ with the 6061 Al substrate. The is distinguished by the Al rich zone. Si is distributed
interfacial region shows the growth of dendrites from uniformly over the entire surface. Table 3 provides
the LMZ towards the coating. the results of the EDS quantitative analysis con-
Fig. 5a. shows the SEM micrograph of the ducted at various locations in the coating. These
cross-section of the coating. TiC particles of various results suggest that the matrix within the coating
size and shape within the matrix of 6061 Al are contains Al 53.24 at.%. and Ti 35.86 at.%. along
observed. The volume fraction of TiC particles in the with some Si 10.88 at.%.. Such high content of Ti
coating is found to be approximately 65%. The in the matrix could possibly be attributed to fragmen-
elemental X-ray maps of the coating corresponding tation andror dissolution of TiC particles. Fragmen-
to Ti, Si and Al distribution are shown in Fig. 5b., tation of such TiC particles is observed in both Figs.
3 and 5a.. Partial dissolution of TiC and, thereby,
availability of free Ti in the matrix is desirable as Ti,
being a highly reactive element, tends to modify the
surface properties of the carbide particles for en-
hanced wettability with the substrate molten mate-
rial. Similar is the case with the interface between
TiC particles and the coating matrix, which contains
Ti 35.19 at.%. along with Al 59.053 at.%. and a
trace amount of Si 5.763 at.%.. Such nature of the
reaction product is expected to provide chemical
bonding in addition to mechanical bonding between
the TiC particles and the matrix.
Fig. 6a. shows the SEM micrograph of the coat-
ing-substrate interface. The corresponding X-ray ele-
mental distribution of Al, Ti and Si is shown in Fig.
6b., c. and d., respectively. Due to a large differ-
ence in the coefficient of the thermal expansions of
metals and ceramics, high residual stresses may oc-
cur at the interface during the rapid solidification
after laser processing. These residual stresses can
Fig. 4. SEM micrograph of LMZ-substrate interface. result in the delaminationrbuckling of the coating
L.R. Katipelli et al.r Applied Surface Science 153 (2000) 6578 71
Fig. 5. a. High magnification SEM micrograph of the cross-section of the coating and corresponding X-ray elemental map of b. Al, c. Si,
and d. Ti.
from the substrate w2x. However, in the present case, Also, interfacial adhesion strength between ce-
no such delamination was observed. This indicates ramic particle and metallic melt is often represented
that the coating is sound and adherent to the sub- by the work of adhesion, Wa , which is defined as
strate suggesting a metallurgical bond. A sharp inter- work per unit area of interface, necessary to separate
face in all these figures suggests no transferrdiffu- reversibly a solidliquid interface to create a solid
sion of Ti into the region of the substrate material vapor interface w27x. Work of adhesion, Wa , for
surrounding the interface. On the contrary, Al has several combination of w28x metalrceramic system is
flown into the matrix of the coating Fig. 6b.. tabulated in Table 4.
The work of adhesion, Wa , reflects directly the
Table 3
importance of energetical interactions between the
EDS analysis in the coating solid and liquid phases. A higher value Wa suggests
Location At.%
stronger interactions w27x. Wa for TiCrSi and
TiCrMg is significantly higher than TiCrAl Table
Ti Al Si
4.. Thus, in the present study, the presence of Si and
Matrix within the coating 35.86 53.24 10.88 Mg in the precursor and 6061 Al is expected to
TiC particles 96.589 0.484 2.927
Interface of TiC particles 35.19 59.053 5.763
increase the wettability and, hence, interfacial
and coating matrix strength between TiC and Al melt, thereby resulting
in an adherent coating.
72 L.R. Katipelli et al.r Applied Surface Science 153 (2000) 6578
Fig. 6. a. SEM micrograph of the coatingsubstrate interface and corresponding X-ray elemental map of b. Al, c. Si and d. Ti.
Table 4
Work of adhesion for metalrceramic systems
Ceramic Metallic Surface energy, g 1y of Contact angle Work of adhesion,
melt liquidvapor interface mJrm2 . in degrees Wa mJrm2 .
TiC Al 914 118 485
Si 860 32 1720
Mg 583 50 960
Fe 1900 39 3578
TiB 2 Al 915 160 55
Si 860 34 1575
Mg Not available Not available Not available
Fe 1785 49 2955
L.R. Katipelli et al.r Applied Surface Science 153 (2000) 6578 73
Fig. 7. a. SEM micrograph of the coating, coatingsubstrate interface, and substrate regions with indentations and corresponding X-ray
elemental map of b. Al, c. Si, and d. Ti.
Fig. 7a. are represented in Fig. 7b., c. and d., low hardness value of LMZ is attributed to the
respectively. The relative difference in size of micro- dissolutionrredistribution of precipitates formed dur-
hardness indentations explains the variation in hard- ing the precipitation hardening of 6061 Al alloy.
ness. Considerably high microhardness values were In the present study, attempts were made to semi-
observed in the coating. The two indentations taken quantitatively determine the interfacial strength. In
in the coating showed different values of microhard- the process, microhardness indentations were made
ness Knoop., with the top part of the coating 572
" 60. relatively harder than the bottom part 454 "
30.. This is due to the presence of SiC, which Table 5
apparently segregated to the top of the coating dur- SEM analysis of the indentations at the interface
ing laser processing. SiC, being less denser 3.1 to Applied Length of the longer SEM predictions
3.2 grcm3 . in comparison to TiC 4.92 grcm3 ., load g. diagonal mm.
floats to the top of molten coating during laser 50 32 No interfacial cracks
processing and remains at the top of the coating after 100 61 No interfacial cracks
resolidification. This fact is also evident from the 200 72 No interfacial cracks
300 107 No interfacial cracks
corresponding X-ray elemental map of Si shown in 500 116 No interfacial cracks
Fig. 7c.. The hardness of the LMZ is 72 " 5 and 1000 150 No interfacial cracks
that of unreacted substrate is 84 " 10. The relatively
74 L.R. Katipelli et al.r Applied Surface Science 153 (2000) 6578
along the interface at various loads 50, 100, 200, SEM micrographs of the indentations taken at all the
300, 500, and 1000 g. to check for initiation of any test loads within the limitations of the indentor being
cracks or delaminations at the site of indentations. used in the present study. SEM observations showed
The loads at which the microhardness tests are con- that there were no visible cracks or delaminations at
ducted and the corresponding SEM observations are these indentations. However, the possibility of fine
illustrated in Table 5. Fig. 8 shows the corresponding stationary cracks within the coating is not ruled out
Fig. 8. SEM micrographs of the indentations taken at the coatingsubstrate interface at various loads.
L.R. Katipelli et al.r Applied Surface Science 153 (2000) 6578 75
since this can only be observed at very high magnifi- study the wear behavior of the coated samples to
cation. The dynamic behavior of these stationary determine the nature of the coating. Fig. 9 shows a
cracks is being further investigated using a four-point plot of weight loss vs. time for the wear tests con-
bending test. Such tests will characterize the strength ducted on TiC coated and uncoated substrate. sur-
of ceramicmetal interface in a quantitative manner. faces of the laser-treated samples. It is clearly ob-
served that the weight loss for the coated side was
3.4. Tribological characterization lower than the substrate side. The wear rate is also
significantly improved. The total duration of the
3.4.1. Wear tests wear test was 20 min. However, while conducting
The tribological performance of a ceramic coating the tests on the uncoated substrate side, the substan-
depends on the characteristics such as hardness, tial weight losses were calculated for a time duration
thickness, internal stress level, and load-bearing ca- of only 30 s due to high seizure of the substrate
pacity. When a coating cools from the high tempera- material during sliding. Comparison of XRD analy-
ture of the melt zone in the deposition process, the ses of the worn and unworn-coated surfaces as illus-
internal compressive stress developed within the trated in Fig. 1 indicated that there are no new
coating reduces the extent of surface fracture and, phases formed during the wear process. This sug-
thus, increases the sliding wear resistance of the gested that the coating was chemically and physi-
coated surface w29x. In addition, wear behavior of cally stable under the dry sliding conditions used in
any material system is expected to be influenced by the present study.
environment, such as dry air or inert atmosphere. Surface roughness profiles shown in Fig. 10a.,
and wet lubricated.. The thermophysical force b. and c. indicated that the average surface rough-
and temperature. conditions at the point of contact ness, R a , of the test sample increased from 0.43 to
are extreme during wear testing. These extreme con- 13.53 mm after laser processing. The average surface
ditions are favorable to cause degradationrdissocia- roughness of the worn surface is 6.51 mm.
tion physical and chemical. of the material and, Topographic features of the worn surface were
hence, occurrence of localized reactions. between analyzed using SEM. Fig. 11a. shows a low magni-
the material and surrounding environment, thereby fication micrograph of the TiC coated 6061 Al sam-
providing different wear responses. ple. X-ray elemental distributions of Al, Ti, and Fe
Wear results in the loss of material, elevation of corresponding to Fig. 11a. are shown in Fig. 11b.,
surface temperature, surface activation, and the re- c. and d., respectively. The worn surface of the
moval of protective film, and, thus, may accelerate coating is identified by continuous wear scars paral-
oxidation or corrosion w30x. Hence, it is important to lel to the laser tracks in some isolated regions of
contact between the sample and wear-disc. During
sliding, there is a material-to-material contact, fol-
lowed by welding or fusing of the contacting asperi-
ties. When sliding continues, the asperities of the
weaker material may shear off and transfer to the
opposite surface w31x. In the present work, the hard-
ened steel sliding disc 62 Rc., whose main con-
stituent is Fe, shears off the Al present as the matrix
of the coating, and Al is collected as the loose debris
at the end of the scars. On the contrary, TiC present
in the coating, being harder than Fe, shears off the
material from the sliding disc, and, as a result, Fe is
deposited in those scars. Such composite nature of
wear and segregation of Al and Fe in particular
regions of the worn surface are clearly seen from
Fig. 9. Weight loss vs. time for the wear tests. Fig. 11a., b. and d., respectively.
76 L.R. Katipelli et al.r Applied Surface Science 153 (2000) 6578
Fig. 10. Optical profilometer figures showing the surface roughness of a. 6061 Al substrate, b. coated side and c. worn coated surface.
3.4.2. Coefficient of friction measurement separation of loose debris from the surface w15x. In
The measurement of the coefficient of friction the present study, the tribometer interfaced with a
provides direct information about the work done to computer recorded the wear test parameters such as
deform the surface of the material. However, it is not Voltage V . and Current I . as a function of time.
necessarily a direct indication of material loss or Based on the principle of energy conservation, the
L.R. Katipelli et al.r Applied Surface Science 153 (2000) 6578 77
Fig. 11. a. SEM micrograph of the worn surface and corresponding X-ray elemental map of b. Al, c. Ti and d. Fe.
frictional force is equal to the electrical work done The frictional theory states that
by the motor given by Wf s m N 9.
Wf s Voltage DV . = Current D I . 8. where N is the normal load, is the linear speed of
the sliding disc and m is the coefficient of friction.
By equating the above equations, the coefficient of
friction can be computed. The computed coefficient
of friction for TiC coating has been plotted for the
entire test time of 20 min as shown in Fig. 12. The
best-fit line shows the coefficient of friction of the
TiC-coated surface to be approximately 0.64.
4. Conclusions
2. The coating is composite in nature with the mi- w10x H.W. Bergmann, Th. Endres, B. Juckenath, LIA 69 1989.
crostructure consisting primarily of hard TiC par- 239, ICALEO.
w11x D. Pantelis, E. Giannetaki, Y. Chryssoulakis, P. Ponthiaux,
ticles reinforced in a matrix of AlTi mixture. Plat. Surf. Eng. 1994. 52.
3. The average surface roughness of the coating was w12x X.B. Zhou, J.Th.M. De Hosson, Acta Metall. Mater. 42 4.
found to be 13.5 mm. 1994. 1155.
4. Considerably high hardness values are obtained in w13x H.J. Hegge, J. Boetje, J.Th.M. De Hosson, J. Mater. Sci. 25
1990. 2335.
the coating.
w14x G.M. Samsonov, I.M. Vinitskii, in: Handbook of Refractory
5. The coating is wear resistant and the wear resis- Compounds, IFI Plenum, New York, 1980, p. 217.
tance is highly influenced by the composite nature w15x A. Agarwal, N.B. Dahotre, J. Mater. Eng. Perform. 8 4.
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6. The coefficient of friction was computed to be w16x JANAF Thermodynamic Tables, 3rd edn. Part-I, AlCo.
w17x R.A. Rapp, X. Zhebg, Metall. Trans. A 22A 1991. 3071.
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w18x J.L. Murray, Metall. Trans. A 19A 1988. 243.
w19x T.Ya. Kosolapova, in: Handbook of High Temperature Com-
pounds: Properties, Production and Applications, Hemisphere
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