Effect of Interstitial Elements on the Welding of Selective Laser Melted Stainless Steel Alloys

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Language: en

00:00:00.800
you
00:00:09.920 00:00:09.930 yeah so as he said I'll be talking about
00:00:12.500 00:00:12.510 the effect of interstitial elements on
00:00:14.299 00:00:14.309 the welding of selectively laser melted
00:00:17.330 00:00:17.340 304 l so this this work is also
00:00:20.720 00:00:20.730 conducted through the NSF iucrc magic
00:00:23.900 00:00:23.910 program and is also sponsored by Los
00:00:26.630 00:00:26.640 Alamos National Lab so it actually
00:00:28.400 00:00:28.410 complements Brandon's Brandon's work
00:00:31.909 00:00:31.919 quite well but we're more focused on is
00:00:34.970 00:00:34.980 once we get a good build what happens if
00:00:38.510 00:00:38.520 you weld it you're essentially putting
00:00:40.460 00:00:40.470 this large macro scale weld on all these
00:00:42.920 00:00:42.930 small micro scale welds and how does
00:00:45.800 00:00:45.810 that affect the weldability in the end
00:00:47.750 00:00:47.760 and you're cracking susceptibility so
00:00:51.910 00:00:51.920 our overall goal of this project is to
00:00:56.090 00:00:56.100 determine the fundamental differences in
00:00:58.510 00:00:58.520 in both gas tungsten arc welding but
00:01:01.130 00:01:01.140 also other processes as well for this
00:01:03.290 00:01:03.300 talk will focus on gas tungsten arc
00:01:05.030 00:01:05.040 welding selectively laser melted 304 L
00:01:09.410 00:01:09.420 and compare that to conventionally
00:01:11.060 00:01:11.070 produce 304 L and more specifically how
00:01:15.170 00:01:15.180 did how does the change in interstitial
00:01:17.120 00:01:17.130 elemental distribution and Composition
00:01:19.670 00:01:19.680 affect the weldability in that sense so
00:01:23.690 00:01:23.700 on the right we have a typical 304 L a
00:01:27.860 00:01:27.870 rot composition was put into thermo-calc
00:01:31.010 00:01:31.020 and you can see it's your your typical
00:01:34.000 00:01:34.010 get your delta ferrite forming first and
00:01:36.740 00:01:36.750 then austenitic structure at the end so
00:01:41.289 00:01:41.299 when we when we effectively changed
00:01:44.719 00:01:44.729 these carbon nitrogen sulfur phosphorus
00:01:47.240 00:01:47.250 which typically affect the weldability
00:01:49.990 00:01:50.000 and now with the 304 l produced by SL m
00:01:55.820 00:01:55.830 with all the powder metallurgy you pick
00:01:58.130 00:01:58.140 up a lot of oxygen so now we effectively
00:02:00.469 00:02:00.479 change our oxygen content and well as
00:02:02.120 00:02:02.130 well and we see that this this graph or
00:02:06.980 00:02:06.990 this Showell simulation plot essentially
00:02:10.759 00:02:10.769 changes and starts to form these panels
00:02:12.920 00:02:12.930 at higher temperatures and eventually
00:02:15.199 00:02:15.209 set up solidifies these manganese
00:02:17.180 00:02:17.190 silicate slags
00:02:18.840 00:02:18.850 towards the end and where do those
00:02:21.720 00:02:21.730 distribute and how do they have
00:02:23.850 00:02:23.860 essentially affect the weldability the
00:02:25.650 00:02:25.660 cracking susceptibility in the end so
00:02:28.920 00:02:28.930 what we did we took some non cracked 304
00:02:33.270 00:02:33.280 L samples made on it yes M to 90 so
00:02:37.260 00:02:37.270 these were done with virgin powder so we
00:02:39.570 00:02:39.580 tried to minimize the amount of oxygen
00:02:41.270 00:02:41.280 and then what we did was we stress
00:02:43.830 00:02:43.840 relieved them for tense at 10 65 for 30
00:02:47.340 00:02:47.350 minutes as per ms 275 9 and so the
00:02:54.210 00:02:54.220 reason we did that was to eliminate the
00:02:56.160 00:02:56.170 effect of residual stress because these
00:02:58.140 00:02:58.150 parts typically have a much higher
00:03:00.150 00:03:00.160 degree of residual stress than the raw
00:03:01.680 00:03:01.690 product so we didn't want that to affect
00:03:03.120 00:03:03.130 the the cracking behavior as we
00:03:06.570 00:03:06.580 previously saw so we we heat treated
00:03:09.090 00:03:09.100 these and then afterwards they were
00:03:10.500 00:03:10.510 machined down to our sample geometry and
00:03:14.030 00:03:14.040 TJ welded and Sigma jig fixture with
00:03:19.320 00:03:19.330 ranging amounts of stress from 0 to 20
00:03:23.430 00:03:23.440 ksi so for those of you that aren't
00:03:27.780 00:03:27.790 familiar with the Sigma tech test is a
00:03:30.030 00:03:30.040 quite old test from the 80s and it's
00:03:35.160 00:03:35.170 actually hot cracking susceptibility
00:03:36.810 00:03:36.820 test which you apply of pre-loaded
00:03:40.320 00:03:40.330 stress onto the sample and perform the
00:03:43.170 00:03:43.180 welding under the stress to try to
00:03:45.360 00:03:45.370 induce the cracking and your cracking
00:03:47.700 00:03:47.710 susceptibility is depending on how much
00:03:49.680 00:03:49.690 stress you need to apply that to induce
00:03:51.600 00:03:51.610 the cracking so this can this is a good
00:03:54.960 00:03:54.970 test for comparing compositional
00:03:57.150 00:03:57.160 variations in between materials so we we
00:04:01.140 00:04:01.150 chose this one as a way to to try to
00:04:05.450 00:04:05.460 determine these differences between the
00:04:07.830 00:04:07.840 am and rock materials so just to give
00:04:11.610 00:04:11.620 you a little bit about the the material
00:04:13.290 00:04:13.300 specifications and the differences in
00:04:14.850 00:04:14.860 composition what we saw was with the the
00:04:18.300 00:04:18.310 SLM we built these samples in two
00:04:21.630 00:04:21.640 different directions so we built them in
00:04:23.940 00:04:23.950 the vertical direction and we also built
00:04:26.460 00:04:26.470 them in the horizontal direction which
00:04:27.960 00:04:27.970 I'll show you schematic in a slider to
00:04:32.140 00:04:32.150 and then we also have our rot material
00:04:34.210 00:04:34.220 there you can see that there's actually
00:04:35.500 00:04:35.510 quite a bit of carving and the rot
00:04:37.870 00:04:37.880 material compared to the to the to the
00:04:41.469 00:04:41.479 am material but in the end the chrome
00:04:44.860 00:04:44.870 and nickel equivalencies are quite
00:04:46.210 00:04:46.220 similar and you see the chrome and
00:04:48.280 00:04:48.290 nickel equivalencies both indicate that
00:04:51.430 00:04:51.440 we'll have a primary ferrite plus
00:04:52.750 00:04:52.760 Austinites location mode upon welding
00:04:54.850 00:04:54.860 and then the major difference that we
00:04:57.610 00:04:57.620 see here is not actually the nitrogen
00:04:59.379 00:04:59.389 which I was expecting since these were
00:05:01.030 00:05:01.040 all built under nitrogen and atomized in
00:05:03.640 00:05:03.650 nitrogen the nitrogen they're actually
00:05:06.070 00:05:06.080 quite a little bit higher in the Sprott
00:05:08.500 00:05:08.510 material but we actually see a tenfold
00:05:13.000 00:05:13.010 increase of the oxygen content in the
00:05:15.490 00:05:15.500 what in the am material compared to the
00:05:17.800 00:05:17.810 rock material so we want to see how that
00:05:20.500 00:05:20.510 how how these specific particular
00:05:22.629 00:05:22.639 elements might affect the cracking the
00:05:27.010 00:05:27.020 am atmosphere was under nitrogen as well
00:05:29.700 00:05:29.710 and we didn't see a significant jump
00:05:33.640 00:05:33.650 spike in the
00:05:39.260 00:05:39.270 not in a significant amount of nitrogen
00:05:41.850 00:05:41.860 no so just show you a little bit about
00:05:51.300 00:05:51.310 the the weld what the weld geometry look
00:05:54.720 00:05:54.730 like we have a typical GTA weld this is
00:05:57.330 00:05:57.340 a two millimeter thick rot material and
00:06:00.180 00:06:00.190 what we do see is this is this skeletal
00:06:04.860 00:06:04.870 ferrite with the mixture of laughy
00:06:07.620 00:06:07.630 ferrite so we do indicate a primary
00:06:09.900 00:06:09.910 ferrite plus austenite structure so the
00:06:13.590 00:06:13.600 WRC predicted quite well
00:06:15.840 00:06:15.850 and we saw that it was it was clean very
00:06:20.130 00:06:20.140 well conducted weld and one thing I do
00:06:22.650 00:06:22.660 want to note because this is important
00:06:24.360 00:06:24.370 for later as we do not see excessive
00:06:26.820 00:06:26.830 oxidation of the surface or the route we
00:06:29.820 00:06:29.830 shielded this with UHP argon both on the
00:06:32.820 00:06:32.830 surface and had a back trail back
00:06:35.130 00:06:35.140 shielding on the root surface as well so
00:06:38.160 00:06:38.170 we try to keep this as clean as possible
00:06:39.930 00:06:39.940 as to not introduce any extra oxygen
00:06:41.940 00:06:41.950 that might skew the results and then so
00:06:48.060 00:06:48.070 when we did the Sigma jig testing of the
00:06:49.740 00:06:49.750 wrought 304 L we see a typical fracture
00:06:54.330 00:06:54.340 pattern as we slowly increase the stress
00:06:56.940 00:06:56.950 I must note that these signatures
00:07:00.030 00:07:00.040 samples the the sample geometry was
00:07:03.110 00:07:03.120 slightly sub sized just because that was
00:07:06.630 00:07:06.640 the build volume that we had for the
00:07:08.400 00:07:08.410 a.m. samples so we had to match
00:07:10.470 00:07:10.480 everything to make it the most
00:07:12.270 00:07:12.280 consistent but we see a slow progression
00:07:14.760 00:07:14.770 of cracking down the centerline as we
00:07:18.060 00:07:18.070 increase the stresses until we finally
00:07:20.580 00:07:20.590 fracture it at 30 ksi and this I believe
00:07:23.430 00:07:23.440 is due to edge effects since we had a
00:07:26.310 00:07:26.320 small smaller sample than the normal
00:07:28.860 00:07:28.870 Sigma jig as far as width goes so it's
00:07:32.820 00:07:32.830 very characteristic of a 304 L nothing
00:07:34.920 00:07:34.930 out of the ordinary
00:07:36.330 00:07:36.340 we had very clean fracture surfaces and
00:07:39.770 00:07:39.780 nothing nothing to cause any alarm so
00:07:44.430 00:07:44.440 then we look at our AM welds so here's a
00:07:48.630 00:07:48.640 schematic of our of our a and Bill's
00:07:51.330 00:07:51.340 both in the horse
00:07:52.350 00:07:52.360 donal direction on the bottom and built
00:07:54.179 00:07:54.189 in the vertical direction on top you
00:07:56.309 00:07:56.319 can't see a change in the weld
00:07:59.670 00:07:59.680 morphology and this could be a product
00:08:03.779 00:08:03.789 of of where where this was cross section
00:08:07.080 00:08:07.090 in the weld this could also be a product
00:08:09.119 00:08:09.129 of compositional variations through the
00:08:12.779 00:08:12.789 build as they were built in different
00:08:14.040 00:08:14.050 directions so but that that didn't that
00:08:19.379 00:08:19.389 didn't necessarily change the fracture
00:08:21.899 00:08:21.909 behavior between the two different sets
00:08:24.029 00:08:24.039 of samples and since they were heat
00:08:25.740 00:08:25.750 treated they were more uniform than in
00:08:29.309 00:08:29.319 the asbill but what we did see where
00:08:31.559 00:08:31.569 small silicate islands in the builds
00:08:33.420 00:08:33.430 themselves so we think that these the
00:08:37.620 00:08:37.630 silicate islands are typically start out
00:08:39.870 00:08:39.880 much smaller and make whoreson during
00:08:41.880 00:08:41.890 heat treatment but we did see a
00:08:44.569 00:08:44.579 scattering of these small silicates that
00:08:46.800 00:08:46.810 you can see in the image on the left and
00:08:49.170 00:08:49.180 in the weld you can see towards the top
00:08:52.410 00:08:52.420 is the or so through the middle as a
00:08:54.990 00:08:55.000 fusion line and towards the top you see
00:08:56.990 00:08:57.000 primary ferrite it's a skeletal ferrite
00:09:00.000 00:09:00.010 solidification so we get primary ferrite
00:09:02.490 00:09:02.500 plus austenite which was also predicted
00:09:04.350 00:09:04.360 through the WRC so that's all good but
00:09:07.889 00:09:07.899 what we did see was a large degree of
00:09:10.829 00:09:10.839 porosity and defects all over the
00:09:12.810 00:09:12.820 material so here on the left you see
00:09:16.490 00:09:16.500 indications of possible ductility
00:09:18.720 00:09:18.730 cracking and you see a large amounts of
00:09:21.420 00:09:21.430 porosity coming to the surface in some
00:09:24.240 00:09:24.250 cases so you can see on the right of
00:09:25.860 00:09:25.870 that left image there's a darker region
00:09:29.189 00:09:29.199 and that's actually an oxide layer that
00:09:31.769 00:09:31.779 had not come off this oxide layer had
00:09:33.960 00:09:33.970 had sort of flaked off but that sort of
00:09:37.680 00:09:37.690 covers up some of the subsurface pores
00:09:39.660 00:09:39.670 that we saw near the surface and then we
00:09:42.810 00:09:42.820 also saw near the towline we're seeing
00:09:44.819 00:09:44.829 the segregation of the silicate that was
00:09:46.769 00:09:46.779 flowing to the towline and forming these
00:09:48.930 00:09:48.940 silicate islands with a mixture of
00:09:51.300 00:09:51.310 spinel in them as well and so we're
00:09:54.030 00:09:54.040 seeing these just decorating the towline
00:09:56.189 00:09:56.199 on either side of the weld four and this
00:09:59.550 00:09:59.560 was consistent throughout all of the
00:10:01.050 00:10:01.060 welds
00:10:03.960 00:10:03.970 and then what we also saw we observed we
00:10:08.490 00:10:08.500 have sort of the silicate formation also
00:10:10.470 00:10:10.480 on the root of the weld so we see this
00:10:13.710 00:10:13.720 thin film in these samples and you can
00:10:17.280 00:10:17.290 also see that the actual towline of the
00:10:19.740 00:10:19.750 weld is a little bit jagged and full of
00:10:23.730 00:10:23.740 these oxide particles and we did again
00:10:26.970 00:10:26.980 use back shielding in argon to try to
00:10:30.630 00:10:30.640 minimize any oxygen and pick up from the
00:10:33.210 00:10:33.220 atmosphere so we didn't oxidize these
00:10:35.790 00:10:35.800 surfaces and this was done under the
00:10:37.980 00:10:37.990 same setup as the raw material so I'm
00:10:40.590 00:10:40.600 very very different at just macroscale
00:10:43.260 00:10:43.270 characteristics that we saw on the
00:10:44.820 00:10:44.830 surface now when we started applying
00:10:47.760 00:10:47.770 loads you see that there's some
00:10:51.600 00:10:51.610 different oxides on the surface but this
00:10:54.720 00:10:54.730 was an unloaded sample there was no
00:10:57.930 00:10:57.940 observed cracking as we started
00:11:00.660 00:11:00.670 increasing the the loads on our turn
00:11:04.740 00:11:04.750 welding we started seeing evidence that
00:11:06.930 00:11:06.940 we may have ductility dip cracking in
00:11:08.850 00:11:08.860 the weld and then we saw a full fracture
00:11:13.770 00:11:13.780 with quite a bit of oxides along the
00:11:16.590 00:11:16.600 fracture line so you can see there in
00:11:18.750 00:11:18.760 the middle there's there's dendrites on
00:11:21.270 00:11:21.280 either side and there's a sort of a
00:11:23.460 00:11:23.470 sharp region where it's a little bit
00:11:25.620 00:11:25.630 darker and with spa EDS analysis we
00:11:29.370 00:11:29.380 indicate high amounts of oxygen content
00:11:31.520 00:11:31.530 manganese and silicon so we saw we saw
00:11:35.190 00:11:35.200 quite a bit of that happening in the
00:11:36.840 00:11:36.850 weld and I'll show you some more images
00:11:38.670 00:11:38.680 on that later and we also observed that
00:11:41.160 00:11:41.170 we had premature and premature
00:11:42.630 00:11:42.640 separations so we only got to 20 ksi
00:11:45.060 00:11:45.070 before these fully fractured so so there
00:11:50.280 00:11:50.290 are quite a few differences there we
00:11:52.230 00:11:52.240 also saw on the surface you could see
00:11:55.110 00:11:55.120 these small dark speckled regions around
00:11:57.330 00:11:57.340 these cracks and those are actually
00:11:59.730 00:11:59.740 these little silicates that had I don't
00:12:02.940 00:12:02.950 know if they had vaporize on the surface
00:12:04.530 00:12:04.540 or had you know sort of floated to the
00:12:06.780 00:12:06.790 surface on these cracks and then we see
00:12:09.570 00:12:09.580 evidence of migrated grain boundaries
00:12:11.100 00:12:11.110 which is why we believe this may be
00:12:13.010 00:12:13.020 ductility dipped cracking occur
00:12:15.369 00:12:15.379 I mean so along the fracture surfaces we
00:12:20.619 00:12:20.629 see these silicate films and you also
00:12:22.210 00:12:22.220 see these large silicate particles that
00:12:26.289 00:12:26.299 are quite irregular and maybe sites of
00:12:28.839 00:12:28.849 initiation for a fracture for premature
00:12:31.929 00:12:31.939 fracture and then we also see an oxide
00:12:33.879 00:12:33.889 coating you could sort of see a dark
00:12:35.559 00:12:35.569 sheen on the right-hand image an oxide
00:12:38.349 00:12:38.359 coating on the dendrites themselves
00:12:40.419 00:12:40.429 along the centerline of the fusion the
00:12:44.829 00:12:44.839 centerline of the weld I'm sorry so we
00:12:47.649 00:12:47.659 think this may be ductility dipped
00:12:49.179 00:12:49.189 cracking Knisley is published a paper on
00:12:54.239 00:12:54.249 the the presence of oxygen and super
00:12:57.219 00:12:57.229 alloys in nickel super alloys may cause
00:13:01.829 00:13:01.839 an increase in ductility dipped cracking
00:13:04.479 00:13:04.489 but it wasn't quantified and this effect
00:13:06.969 00:13:06.979 has not been studied another another
00:13:09.189 00:13:09.199 sample so we think that this might be
00:13:12.729 00:13:12.739 since we're under high restraint we
00:13:14.949 00:13:14.959 think this might be a product of
00:13:17.829 00:13:17.839 ductility dipped cracking for some of
00:13:21.099 00:13:21.109 those some of the fracture mechanisms as
00:13:23.889 00:13:23.899 well as solidification cracking at
00:13:25.599 00:13:25.609 higher and higher stresses so that's
00:13:28.749 00:13:28.759 something that we need to look into
00:13:30.509 00:13:30.519 quite a bit more and since we have these
00:13:33.429 00:13:33.439 high these oxidizing elements such as
00:13:37.269 00:13:37.279 manganese silicon and Chrome they tend
00:13:40.059 00:13:40.069 to pick up all that extra oxygen and as
00:13:43.119 00:13:43.129 well we already have these silicate
00:13:44.590 00:13:44.600 particles in them in the sample itself
00:13:47.229 00:13:47.239 before we weld so we might just be
00:13:48.999 00:13:49.009 redistribute them into the weld and
00:13:52.379 00:13:52.389 forming these cracking initiation sites
00:13:56.249 00:13:56.259 so to conclude the the oxygen inherent
00:13:59.079 00:13:59.089 to the the 3d printing process it may
00:14:01.929 00:14:01.939 pose a detrimental effect to a
00:14:06.899 00:14:06.909 detrimental occurrence of cracking
00:14:09.689 00:14:09.699 premature cracking compared to the
00:14:11.919 00:14:11.929 wrought material we do need is a study
00:14:14.589 00:14:14.599 this quite a bit more and figure out
00:14:16.539 00:14:16.549 exactly what's happening and if this was
00:14:19.029 00:14:19.039 a product of these builds themselves or
00:14:21.009 00:14:21.019 if this is a product of other batches of
00:14:23.019 00:14:23.029 builds and also study other other
00:14:29.329 00:14:29.339 types of welding to compare this
00:14:31.449 00:14:31.459 phenomena and we did see an increase of
00:14:34.970 00:14:34.980 cracking susceptibility between these
00:14:36.800 00:14:36.810 SLM samples compared to the rot so I
00:14:39.199 00:14:39.209 think this is definitely an issue that
00:14:40.819 00:14:40.829 needs to be addressed and looked into
00:14:42.889 00:14:42.899 quite a bit more and determine what
00:14:46.249 00:14:46.259 these act these mechanisms actually are
00:14:48.259 00:14:48.269 causing this premature failure
00:14:52.720 00:14:52.730 [Applause]
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