4.1. Weld Profiles and Defects
Typical EB weld profiles for both rolled and L-PBF’ed samples are shown in Figure 5. As expected, E-beam can penetrate very deep in metal and provide excellent weld penetration. The top of a weld had a wide ‘nail-head’ shape which gradually reduced in width to a slender ‘nail-point’ shape at the bottom. The large weld volume of a nail-head was seen at beam entrance since this volume was subjected to the larger effective beam diameter of the focusing beam, and longer beam exposure time. A higher heat input of the beam allowed larger weld volume and deeper penetration. Full penetration of the 13 mm rolled plate is shown in Figure 5 when the heat input was 259.3 J/mm and the welding speed was 660mm/min (sample A1). Voids (keyholes) were observed at the bottom of the welds due to fast welding speeds as seen in samples A4 (247.6 J/min, 787.4 mm/min) and A7 (213.2 J/mm, 914.4 mm/min) but not on other samples. Similar voids occurred at the welded bottom of L-PBF samples (Figure 6 (a)), and additional voids were found near the HAZs of the weld head (Figure 6 (b)). No similar voids were found at the nail head of the rolled samples welded at the same E-beam parameters. Thus, it was postulated that the voids at the nail head originated from pores /defects in L-PBF and worsened due to solidification shrinkage of the molten metal in the weld. This hypothesis was further supported by observations in the twin samples where no void was seen. Both rolled samples A8 (and its twin) and L-PBF sample 18A (and its twin) showed no void in the weld joined at low 196.8 J/mm heat input.
Figure 7 and Figure 8 respectively show the linear dependency of weld penetration depth on heat input and weld area (excluding void area) against the beam current. A slow beam speed allowed more interaction time between the beam and the material, and therefore, formed a larger molten volume and weld area. Deeper penetration was found for rolled samples as compared to L-PBF’ed samples at the same heat inputs. Since the beam accelerated voltage was kept constant at 50kV, the weld area also increased with higher heat input.
4.2. Tensile properties
When fabricating the tensile specimens, any pores and defects on the top and bottom of a weld were machined away to reduce the 13mm thick sample to 6mm per the ASTM E8 standard. Thus, the welded specimens in this study simulated the ideal scenario when separated workpieces were perfectly aligned and then welded for through-thickness penetration. All the L-PBF’ed welded samples were fractured at the weld except for the sample 16A. Both the as-printed samples (20A-B) were broken away from the center of the specimens. Figure 9 plots typical stress-strain curves of the welded L-PBF’ed twin samples (19A-B); similar plots for the rolled IN718 twin samples (A91-2) are superimposed for comparison.
Table 4
Mechanical Properties of EBW’ed L-PBF IN718 samples
Sample Label
|
EBW Heat Input
(J/mm)
|
YS
(MPa)
|
UTS
(MPa)
|
Young’s Modulus
(GPa)
|
Ductility
(%)
|
Toughness
(J/mm3 x 10-3)
|
11A/B
|
295.3
|
720, 722
|
937, 998
|
10.9, 10.5
|
16.9, 22.5
|
102, 155
|
12 A/B
|
272.6
|
715, 724
|
925, 987
|
11.0, 10.5
|
17.0, 20.6
|
98, 143
|
13 A/B
|
249.8
|
722, 703
|
951, 1004
|
10.8, 10.4
|
19.1, 22.3
|
117, 161
|
14 A/B
|
247.6
|
714, 724
|
899, 967
|
10.9, 10.7
|
15.1, 18.2
|
85, 102
|
15 A/B
|
228.6
|
737, 706
|
976, 932
|
10.9, 10.6
|
19.5, 16.8
|
125, 103
|
16 A/B
|
209.6
|
724, 709
|
889, 931
|
10.7, 11.6
|
15.8, 16.4
|
87, 102
|
17 A/B
|
213.2
|
719, 712
|
927, 899
|
10.9, 10.8
|
18.8, 13.4
|
125, 75
|
18 A/B
|
196.8
|
702, 708
|
891, 888
|
10.7, 11.2
|
16.5, 14.0
|
88, 77
|
19 A/B
|
180.4
|
735, 710
|
1004, 953
|
10.9, 11.1
|
22.7, 17.5
|
159, 110
|
20 A/B
|
-
|
741, 745
|
1045,1024
|
10.8, 10.9
|
28.1, 27.7
|
210, 198
|
At the same EB welding parameters, it was found that:
-
The stress-strain curves of twin samples repeated very well.
-
The yield and tensile strengths of L-PBF’ed samples were higher than those from the rolled samples
-
The ductility and toughness (area under stress-strain curve) of typical L-PBF’ed material, however, were less than those of the rolled material.
Table 4 summarizes and compares tensile properties for each twin pair of L-PBF’ed and rolled samples. Recall that the twin samples 20 A-B were printed by L-PBF but not subjected to EBW.
Figure 10, Figure 11, and Figure 12 below plots and compares the mechanical properties of EB-welded samples of rolled or L-PBF’ed materials. The data show that:
-
All L-PBF’ed samples exceeded the minimum yield strength of 600MPa, specified in the ASTM F3055-14a standard for additively manufactured IN718. The yield strengths of L-PBF’ed samples also exceeded those of the rolled samples (Figure 10).
-
When comparing the tensile strength, at least one replicate of each sample exceeded 920MPa, specified in the ASTM standard, except for sample 18A-B (196.8 J/mm). Again, all the tensile strength of L-PBF’ed samples exceeded those of their rolled counterparts (Figure 11).
-
All the EBW’ed L-PBF samples had low ductility, therefore, they neither met the ASTM standard nor could compare to the ductility of the rolled samples (Figure 12). The as-printed samples (20A-B) with 27.7-28.0 % elongation was marginally met the ASTM standard requirements for elongation (27%) but were inferior to that of the rolled samples. The brittleness of L-PBF samples can be explained by the resulted microstructures that are presented in the fractography section.
4.4. Fractography
Analysis of fractured surfaces reveals useful information that explains the tensile properties of tested samples. This section presents fractured surfaces of selected L-PBF’ed and rolled samples and compares the fracture surfaces inside and outside of corresponding welds. Figure 14 shows the SEM images of the fractured surface of rolled EBW sample A81 (196.8 J/mm) that broke outside the weld. Fracturing outside of a weld zone indicated the success of the EBW’ed samples at optimal welding parameters. Isolated dark and brittle particles were seen throughout the surface. Recall that the chemical composition of IN718 materials in this study (Table 2) was within the ASM specifications. The EDS spectrums (Figure 15) of a zone outside of such particle confirmed the correct chemical composition of IN718, however, analysis of points on the particle showed excessive niobium (Nb), carbon (C), and titanium (Ti) contents with a reduced amount of nickel (Ni) and chromium (Cr). Such (Nb, Ti, C) intermetallic compounds degraded the material. Although the number of these brittle particles, and its volumetric density, were relatively small to significantly affect the tensile properties, they were the crack nucleation sites that certainly degraded the fatigue and creep property of such a sample.
Figure 16 shows the fractured surface inside the weld zone of the rolled sample A21 (272.6 J/mm). Very fine grains were seen due to the fast cooling of the small weld surrounded with a larger volume of the parent material. Isolated (Nb, Ti, C) brittle particles were visible inside the ductile matrix as confirmed with EDS analysis.
Fractured surface of the as-printed L-PBF’ed sample 20A revealed evidence for the low ductility of this sample. The fracture occurred away from the gage center (weld zone) when confirmed with chemical etching to reveal the weld zone at the specimen center. Defects on the surface (Figure 17) include:
-
Un-melted IN718 powder particles and unfilled zones (Figure 17 (a)). These stress-raiser sites would degrade the mechanical properties of L-PBF’ed materials.
-
Large chunks of brittle phases with irregular shapes were plentiful on the surface (Figure 17 (b)). EDS analysis confirmed the Nb-rich content of the Laves phase.
Figure 18 (a) shows the fractured surface of L-PBF’ed sample 17A that broke inside the weld. The very-ductile matrix was evidenced with dimple fracture surface and fine grains. Distinct brittle features of some particles were seen. The EDS analysis at different locations (Figure 18) showed the weight percentage of Nb in the ductile matrix was normal for Nb (4.7 %, that is nearly within the 4.74-5.5% from ASM specification) and Al (0.7%, that is within the 0.2-0.8% from ASM specification). However, the levels for Nb (6.1-9.9%) and Al (1.0-3.2%) of brittle particles were much higher than the maximum chemical levels from the ASM allowance. This confirmed that those brittle particles were the Laves phase and consistent with published literature.
Figure 19 shows other defects inside the weld of sample 17B: the fractured of gas-filled spherical pores (Figure 19 (a)) that served as sites with high stress concentration; an un-melted spherical particle that was delaminated from the ductile matrix (Figure 19 (b)). Although the shape and size of the powder in Figure 19 (b) was similar to the virgin IN718 powder particle, it must be a different material since it was not melted and has no bond to the surrounding IN718 matrix.
At a different location on this sample, a remnant of a brittle spherical particle is shown in Figure 20(a). The EDS analysis (Figure 20 (b)) of this particle showed the unusual chemical compositions of oxygen (49-51.4%), aluminum (35.6-37.7%), and titanium (7.3-9.6%) as compared to those from the surrounding materials (0% oxygen, 0-0.6 aluminum, and 0-1% titanium). It was assumed that the spherical particle in Figure 20 (a) was similar to that in Figure 19 (b) when comparing the shape, relative size, and similar delamination from the matrix. Since aluminum oxide (Al2O3) has 52.9% Al and 47.1% O, the spherical particle in Figure 20 with 35.6-37.7% Al and 49-51.4% O are not aluminum oxide but an (Al, Ti, O) compound. However, Popovich et al. [20] studied different heat treatments of IN718 and reported the finding of brittle aluminum oxides.
When studying the fractured surface of sample 16A1, addition defects were found that caused it to fracture outside of its weld zone. Large zones of delaminated layers were seen (Figure 21 (a)) perhaps due to inadequate heat input of 209.6 J/mm. Remnants of spherical pores (Figure 21 (a)) and scattered of brittle Laves phases were also observed (Figure 21 (b)).
Both the L-PBF and EBW processes melt and solidify affected materials at different cooling rates. Solidification of IN718 underwent three stages [22]:
1. Firstly, the liquid phase transformed into the secondary γ phase and led to precipitation of solute particles such as Nb, C, Ti, in the interdendritic region.
2. Secondly, the segregation of the particle led to the formation of intermetallic carbides. All or most percentages of carbon in the alloy were consumed in this process; the higher the percentage of carbon in the base alloy matrix, then the higher was the tendency of the carbide formation.
3. Thirdly, further enrichment of the solute led to the formation of the Laves phase (Figure 17 (b), Figure 18 (a), and Figure 21 (b)) before the ending of the solidification process.
The formation of the Laves phase was directly proportional to the presence of segregated niobium. The Nb segregation depended mainly on the cooling rate of the molten alloy. A higher cooling rate would lower the segregation of niobium [23]. Thus, favorable material characteristics can be observed at high cooling rates during L-PBF or EBW. Niobium presence in the alloy solution was shared by various secondary phases (δ, γ, γ’, and γ’’) during solidification. Thus, the higher percentage of any of these phases led to a more reduction in the percentage of the others. In the case of weld-zone, percentage of the strengthening phase γ’ and γ’’ was reduced due to high consumption of Nb by the δ and γ phases [9, 21]. Further, the formation of Laves and δ phase in the grain boundaries provide favorable sites for nucleation of voids and fissures. This led to poor mechanical properties and hardness of the welds as compared to that of the base metal. Further, the presence of un-melted particles, voids, pores, and oxides that prevent adhesion between adjacent layers contribute to brittleness in L-PBF’ed parts. In summary, the low ductility of welded L-PBF’ed IN718, measured in tensile testing, was due to:
-
Un-melted powder particles and lack of fusion in L-PBF’ed samples (Figure 17 (a)).
-
Inevitable gas-filled spherical pores (Figure 19 (a)).
-
Delamination of an un-melted spherical powder and the surrounding matrix (Figure 18 (b)).
-
Brittle Laves and other phases (Figure 17 (b)).
-
Unfavorable size and distribution of precipitates.
The L-PBF process-induced thermal gradients between adjacent layers thereby fusing them and leading to a formation of homogenous metal in an ideal case. Uneven layer thickness, fluctuation of laser power, powder contamination can form gaps between the adjacent layers (Figure 21 (a)). This led to inadequate heat distribution and left some powder particles un-melted (Figure 17 (a)). Spherical pores were also observed throughout the samples (Figure 17 (a) and Figure 21 (a)). Porosity can be formed due to various mechanisms [24]:
-
Presence of voids between the partially melted powder particles,
-
The collapse of molten pool depression due to high scanning speeds,
-
Denudation of un-melted particles surrounding the laser beam path, and
-
Impartial melting and fast cooling at the end of the laser path on a layer.
Towards the end of the scanning path, the beam quickly changed direction, or turned off, leading to the reduction of temperature at the molten surface at the end of the path, thus (i) increased the molten material viscosity, (ii) hindered the flow of molten metal, and (iii) led to a formation of the void at the center of the melt pool. This explained the presence of voids towards the edge of the L-PBF’ed samples. The same mechanism also explained the presence of voids at the HAZ or boundary of the EBW fusion zones. Keyhole defects at the bottom of the welds with high heat inputs also occurred due to the same mechanism [10].