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Article history: In the current investigation AISI 4340 steel was laser deposited on a rolled mild steel substrate by Direct
Received 23 September 2010 Metal Deposition (DMD) technology. The microstructural investigation of the clad was performed using
Received in revised form 2 November 2010 optical and electron microscopes and X-ray diffraction techniques. The microstructure consisted of ferrite,
Accepted 9 November 2010
martensite and cementite phases. Two types of martensite, lathe-type and plate-type, were observed in
Available online 16 November 2010
the microstructure. Decrease in microhardness values from the top layer to the alloy layer proves that the
degree of tempering of the martensite phase increases in the same direction. The lattice parameters of
Keywords:
the identified phases were found to be shorter than those reported in literature. The reported parameters
Direct Metal Deposition
Clad
in literature are from samples processed under equilibrium conditions.
Microhardness © 2010 Elsevier B.V. All rights reserved.
Tempering
Lattice parameters
0921-5093/$ – see front matter © 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2010.11.036
2310 S. Bhattacharya et al. / Materials Science and Engineering A 528 (2011) 2309–2318
Fig. 1. SEM micrograph of AISI 4340 steel powder showing (a) particle morphology (b) particle cross-section.
AISI 4340 steel is a medium carbon, heat treatable, high strength cross-section can be seen in the SEM micrograph of Fig. 1(b). The
low alloy (HSLA) steel used for critical structural applications, such powder particles were mostly spherical with an average parti-
as building components, automobile components, high pressure cle size of 75 m and 85% of the particles within the 60–120 m
vessels for nuclear power plants, and aircraft components, due to its range. Approximately 100 particles per micrograph were selected
toughness, high strength and ability to retain good fatigue strength for measurements and always the largest diameter and the diame-
at elevated temperatures [11–13]. The microstructure of carbon ter in the direction perpendicular to the long axis were measured.
steels primarily consists of a mixture of ferrite with some cementite The average powder particle porosity was found to be approxi-
carbides, tempered and untempered martensite, and some retained mately 0.45%.
austenite depending on the processing conditions. Primary alloy-
ing elements (nickel, chromium and molybdenum) addition along 2.2. Sample preparation
with carbon makes it the material of choice for corrosion and wear
resistant applications, e.g. for making medical devices (along with Fig. 2 shows the schematic of DMD process. DMD system primar-
stainless steels) and submarine components used under submerged ily consisted of the laser generation system, the powder delivery
conditions [13,14]. system, feedback control system, and CNC motion stage [16]. The
The current research effort was undertaken to evaluate the DMD process could be performed either in air or under controlled
microstructure evolution during the repair of some high value AISI atmosphere. DMD samples for this investigation were prepared
4340 steel components by DMD process. AISI 4340 steel has been at Focus: HOPE using a 1 kW fiber coupled diode laser (Laserline
well researched. However, reported literature on laser processing GmbH, Germany) POM DMD 105D system with a 2 mm diam-
of AISI 4340 steel primarily discuss laser surface treatment and its eter laser beam. A combination of DMD processing parameters:
effect on the mechanical properties of the alloy. Few published laser powers 500, 550 and 600 W, processing speeds 400, 450, and
works have also reported the microstructural characterization of 500 mm/min, and powder feed rate 5, 6 and 7 g/min and 50% over-
post laser treated AISI 4340 steel surfaces [12,13,15]. In this inves- lap between two adjoining passes, were used to build a trial sample
tigation complete microstructural characterization and mechanical matrix (Table 2), and later experimental samples. Argon was used
properties (based on microhardness measurements), of AISI 4340 as both carrier and shielding gases during deposition. The trial sam-
steel deposited by DMD process has been reported, which is not ple matrix was made to perform a statistical design of experiment
available in open literature. The paper also investigates the change (DOE) based on a L9 orthogonal array of Taguchi method [17] in
in lattice parameters of the microstructural phases due to rapid order to optimize parameters to produce samples with minimum
solidification. porosity and maximum deposition rate. Table 3 shows the opti-
mal parameter combination drawn from this trial sample matrix
2. Experimental
2.1. Materials
Table 1
AISI 4340 steel powder composition (wt.%).
Fe C Ni Cr Mn Mo Si
Bal. 0.42 2.63 0.90 0.74 0.45 0.29 Fig. 2. Schematic diagram showing the DMD process.
S. Bhattacharya et al. / Materials Science and Engineering A 528 (2011) 2309–2318 2311
Table 2
DOE sample matrix used for developing process parameters for AISI 4340 steel on mild steel substrate using diode laser.
Run order Power (W) Scanning speed (mm min−1 ) Powder feed rate (g min−1 ) Deposition quality Average porosity (%)
Fig. 3. Optical micrograph showing the longitudinal cross-section of the experimental sample and a diagram showing the laser scanning direction and layers in AISI 4340
steel DMD sample.
2312 S. Bhattacharya et al. / Materials Science and Engineering A 528 (2011) 2309–2318
3.1. Microstructure
3.1.2. Scanning electron microscopy
Fig. 4 shows three-dimensional view of microstructures at three
Specimens for OM, SEM and MH measurements were cut from
different locations along the clad; (a) first few layers, (b) middle
different parts of the experimental sample and etched with 2.5%
layers, and (c) top layers. Fig. 5(a–h) shows the longitudinal (x–z)
Nital (97.5% ethanol and 2.5% nitric acid) solution to reveal the
view microstructures of clad layers 7 through alloy layer. Fig. 5(i)
microstructure.
shows the interface microstructure, and Fig. 5(j) shows the sub-
strate microstructure.
3.1.1. Optical microscopy Fig. 6 shows the plan (x–y) view microstructure of the clad.
Fig. 3 shows the optical micrograph of the longitudinal (x–z) The longitudinal view microstructures clearly show needle shaped
cross-section of the as-deposited experimental sample, and a martensite in the top few layers (layer 7–5), and they appear to get
schematic of the laser deposition and laser scanning directions tempered or rounded in middle through lower layers (layer 4–1),
in different clad layers. Total thickness of the clad was found to towards the interface. The grain size also appears to increase in
be approximately 3.400 m. Thickness of each layer was found to that direction. Plan view (Fig. 6(b)) also shows microstructure with
vary approximately between 300 m and 500 m. However, no probably some retained austenite along the grain boundaries. How-
feedback control was used during these experiments. Since the Z ever, XRD and TEM analysis did not detect any retained austenite
increment for each layer during deposition was kept constant at phase.
0.5 mm (500 m), it shows that there is some interlayer overlap Fig. 5(j) shows typical rolled microstructure with large grains in
during deposition. The laser band width measured from optical the substrate. Interface and alloy layer also show some fine tem-
micrograph (Fig. 3) was found to be approximately 943 m. Also pered martensite and larger grains. Fig. 7 shows the EDAX® analysis
as the laser beam diameter was 2 mm (2000 m), percentage over- of the clad layers and Table 4 gives the chemical composition
lap measured from optical micrograph was approximately 50%. The of the clad obtained from the analysis. The chromium composi-
Fig. 4. SEM micrographs showing the three-dimensional view of the AISI 4340 steel DMD sample at three different locations (a) first few layers, (b) middle layers, (c) top.
S. Bhattacharya et al. / Materials Science and Engineering A 528 (2011) 2309–2318 2313
tion in the clad was found to be slightly higher than the powder room temperature. Since DMD is a non-equilibrium process some
composition. metastable phases such as martensite could be certainly expected
in the microstructure.
3.1.3. X-ray diffraction analysis
Fig. 8 shows the XRD plot of the AISI 4340 steel DMD clad. 3.1.4. Transmission electron microscopy
Ferrite (␣-Fe), martensite, and cementite (Fe3 C) phases were iden- Figs. 9(a), 10(a) and 11(a) shows the bright field (BF) images of
tified from the plot. No retained austenite was observed in the microstructural phases and Figs. 9(a), 10(a) and 11(a) shows their
XRD plot. The equilibrium microstructure of hypo-eutectoid steel is corresponding selected area diffraction (SAD) patterns. SAD pat-
expected to be primarily ferrite and pearlite (ferrite + cementite) at terns identified these microstructural phases, i.e. ferrite, martensite
Fig. 5. SEM micrographs showing longitudinal (y–z) view microstructures of the AISI4340 DMD® sample layers (a) through (h) corresponding to layer 7 through alloy layer,
(i) interface, and (j) substrate marked in Fig. 3.
2314 S. Bhattacharya et al. / Materials Science and Engineering A 528 (2011) 2309–2318
Fig. 5. (Continued.)
and cementite and corroborated the XRD results. Retained austen- pattern peaks (PDF #00-044-1290) were reported as 2.859 Å and
ite phase was not detected in TEM investigation as well. The phase 2.937 Å,respectively. The corresponding calculated lattice parame-
identified from the SAD pattern of Fig. 9(b) was ferrite (␣-iron), ters from SAD pattern were 2.856 Å and 2.902 Å, respectively, which
with a body centered cubic (BCC) crystal structure and a [0 1 1] were approximately 0.1% and 1.2% shorter than the reported val-
zone axis (ZA). Lattice parameter a of the ferrite phase match- ues. The phase identified from the SAD pattern of Fig. 11(b) was
ing the XRD pattern peaks (PDF #04-004-2482) was reported as cementite (Fe3 C), with an orthorhombic crystal structure and a
2.8676 Å. The corresponding lattice parameter calculated from the [0 0 1] ZA. The reported lattice parameters a, b and c of the cemen-
SAD pattern was found to be 2.810 Å, which was approximately tite phase matching the XRD pattern peaks (PDF #01-074-3832)
2.0% shorter than the reported values. The phase identified from the were 4.5119 Å, 5.0825 Å, and 6.7330 Å, respectively. The corre-
SAD pattern of Fig. 10(b) was a lathe type martensite with a body sponding calculated lattice parameters from the SAD pattern were
centered tetragonal (BCT) crystal structure and a [1̄ 1 1] ZA. Lat- 4.4800 Å, 5.0509 Å, and 6.7291 Å, which are approximately 0.7, 0.62
tice parameters a, and c of the martensite phase matching the XRD and 0.058%, respectively shorter than the reported values. The lat-
Fig. 6. SEM micrographs showing the plan (x–y) views microstructure of the AISI 4340 steel DMD® sample.
Fig. 7. EDAX analysis showing chemical composition of the AISI4340 DMD® clad.
S. Bhattacharya et al. / Materials Science and Engineering A 528 (2011) 2309–2318 2315
4. Discussion
Fig. 9. (a) Bright field image showing the area marked for SAD in the ferrite phase (␣) and (b) corresponding indexed SAD pattern.
Fig. 10. (a) Bright field image showing the area marked for SAD in the martensite phase (m) and (b) corresponding indexed SAD pattern.
2316 S. Bhattacharya et al. / Materials Science and Engineering A 528 (2011) 2309–2318
Fig. 11. (a) Bright field image showing the area marked for SAD in the cementite (Fe3 C) and (b) corresponding indexed SAD pattern.
Fig. 12. Bright field image showing (a) martensite and dislocation networks around martensite.
DMD usually are as high as 103 –105 K/s [7,13] and result in devi- consists of secondary phases, such as several alloy carbides [19]
ation from equilibrium microstructure. CCT diagram shows that depending on the composition.
extremely rapid cooling rates place the DMD process to the extreme The microstructural investigation of DMD AISI 4340 steel, using
left hand side of the diagrams, below the martensite finish line. The SEM and TEM, reveals that the clad primarily consists of ferrite
DMD microstructure of an alloy steel is thus expected to be pri- and martensite and some cementite phases. According to Costa
marily martensitic. The microstructure of the alloy steels may also and Vilar [20] extremely rapid cooling rate during DMD suppresses
the diffusive microstructural transformations and results in major-
Fig. 13. Plot showing variation microhardness with distance from interface. Fig. 14. Plot showing microhardness measured along each layer.
S. Bhattacharya et al. / Materials Science and Engineering A 528 (2011) 2309–2318 2317
Fig. 15. (a) Portion of the Fe–C equilibrium phase diagram showing the equilibrium phases present at the sample composition indicated by an arrow [18] and (b) continuous
cooling transformation (CCT) diagram for alloy steel [18] (A = austenite, B = bainite, F = ferrite, M = martensite, P = pearlite).
ity of carbon atoms to remain in the solution in austenite (␥-Fe) ical properties of the material could be directly related to the crystal
phase and form metastable martensite phase. The carbon atoms structure of each phase [24]. Researchers have [25,26] investi-
occupying the interstices in the BCC lattice in ferrite phase causes gated the effect of residual stress on the mechanical behavior of
distortion of the lattice in one direction while contraction in the microstructural phase in materials. The effect of cooling rate on the
other two normal directions and thus resulting in a BCT structure. microstructural phases is observed in the TEM SAD patterns. The
The strength of the martensitic structure in steels depends on the lattice parameters of the phases identified using TEM SAD patterns
tempering temperature, carbon content and the martensite start were shorter as compared to the lattice parameters for the same
(Ms ) and finish (Mf ) temperatures [21]. Lee and Su [22] related the phases reported in literature. The reported lattice parameters were
change of martensite morphology with carbon content. They stated obtained from the samples with equilibrium processing. This shows
that low-carbon content results in lathe type martensite with high the effect of residual stresses present in DMD clads on the crys-
density of dislocation, as observed in rolled structure, high carbon tal structure of the microstructural phases. No information on the
content results in plate type martensite with very fine twins and effect of residual stresses on lattice parameter of microstructural
medium carbon content results in a complicated microstructure phases is available in open literature.
with a mixture of lathe and plate type martensite. Figs. 11 and 12 Fastow et al. [15,27] reported the presence of traces of
shows that the both lathe and plate types of martensite are present retained austenite phase along with martensite phase in the
in the current DMD AISI 4340 steel samples microstructure of laser surface alloyed AISI 4340 steel. Researchers
Heat treatments can alter the distribution, size and morphol- [28,29] have also reported the presence of retained austenite
ogy of the metastable phases and also results in the precipitation phase on prior austenite grain boundaries in cast and laser
of secondary phases [22,23] in as-cast structure. Lee and Su [22] surface treated AISI 4340 steel samples. Sastry and Wood
showed that the cast microstructure of AISI 4340 steel consisted [28] showed that the orientation between retained austen-
of lathe martensite and tempering process resulted in the growth ite and martensite exhibited a Kurdjumov–Sachs relationship,
of the lathes and precipitation of several types of carbides around (1 1 1)␣ //(1 1 0)␥ in a laser surface treated AISI 4340 steel sam-
these lathes. During DMD a considerable amount of heat is trans- ple. Molian [29] showed that cementite particles precipitated
ferred to the bulk, hence starting from substrate every layer acts during heat treatment of cast AISI 4340 steels displayed Bha-
as a heat sink for the subsequent layers above it. Thus according garyatskii orientation relationship with martensite such as,
to Costa and Vilar [20] every solidified layer undergoes successive [0 1̄ 1]␣ //[1 0 0]Fe3 C , [1 1̄ 1]␣ //[0 1 0]Fe3 C and (2 1 1)␣ //(011)Fe3 C .
thermal cycles as new layers are deposited and results in solid- SEM micrographs (Fig. 6) also show some retained austenite along
state microstructural transformation in these resolidified layers. the grain boundaries in the current sample. However, they were
This could significantly change the matrix microstructure, distribu- neither detected in XRD scans nor in TEM analysis. These orien-
tion of secondary phases and eventually material properties [22]. tation relationships between austenite (␥), ferrite (␣), martensite,
SEM micrographs (Fig. 5) show that the martensite phase in layer -carbide and Fe3 C phases in DMD AISI 4340 steel deposited using
7 is fine needle shaped and it gets tempered and rounded in sub- a CO2 laser have been explored in detail by our group in another
sequent layers towards the interface. The microstructure of lower publication [30].
layers is etched darker as compared to upper layers. Decrease in It was found that the formation of martensite from ␥
microhardness values (Figs. 13 and 14) from layer 7 to alloy layer followed the conventional Kurdjumov–Sachs relationship. Orien-
also proves that the degree of tempering of the martensite phase tation relationship between -carbide and Fe3 C also followed the
follows same direction. conventional orientation relationships reported in literature. How-
Extremely rapid cooling during DMD results in residual stress ever, the relationship between ␣- and -carbide did not follow any
accumulation in clads [9]. These residual stresses could affect the of the conventional orientation relationships reported in literature
crystal structure of microstructural phases in the clad. The mechan- [30].
2318 S. Bhattacharya et al. / Materials Science and Engineering A 528 (2011) 2309–2318