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ELECTROPOLISHED TUBING
by
Sunniva R. Collins
Research Metallurgist
and
Peter C. Williams
Chief Scientist
Swagelok
×
Figure 1 Acceptable and rejectable weld at approximately 10×
Introduction A AF FA FA F
AISI 316L is commonly used in many
industries, including the bioprocess or L L L L L
pharmaceutical industries, in fluid system
applications. In these applications, large systems
of AISI 316L tubing are orbitally/autogenously
welded in place. As a method of construction,
welding is fast and avoids the crevices (and
potential for crevice corrosion) common with
mechanical couplings. Unacceptable weld
characteristics include bead meander, oxidation, L = liquid = austenite = ferrite
and slag formation. There are also cosmetic
geometric issues, such as weld bead width and Figure 2 Solidification Modes in AISI 316L
height. A = austenitic; AF = austenitic-ferritic; FA =
ferritic-austenitic; F = ferritic
In bioprocess applications, cleaning in
place (CIP) is common. The systems must avoid occurs when aerobic and anaerobic microbes
corrosion in service, as corrosion products will create a colony by removing material, forming
contaminate the final product. Bioprocess deep pits with small pinhole openings on the
applications are usually wet, which introduces interior of the tube. MIC in a system can speed
the possibility of rouging and microbially up corrosive processes drastically; a system
induced corrosion. Rouge is a contaminant designed to work for 10 years can fail in two or
found in many hot water and steam systems less if MIC is present.
consisting of various forms of iron oxide; these
Weldability of 316L
iron oxides are a corrosion product that can
affect the purity of the final product. Rouge is Compositional restrictions on 316L have
often treated in by shutting down, cleaning and been explored, particularly on residual or tramp
repassivating the entire system. Microbially elements.(1) Many of these restrictions have to do
induced corrosion initiates in the heat affected with the slag that may form on welds, or the
zones of welds, and in crevices or cracks. MIC redeposited metallic vapors that may potentially
WELDABILITY AND CORROSION STUDIES OF AISI 316L ELECTROPOLISHED TUBING
by Sunniva R. Collins and Peter C. Williams
Table 2. Weldability Testing: Test Matrix of 2.0-in. diam. 316L Electropolished Tubing, wt %
Heat No. Cr Mo Si Nb Ti Ni Mn C N Cu P S
1 16.8 2.1 0.4 0.011 0.01 10.22 1.82 0.012 0.052 0.3 0.026 0.011
2 16.92 2.06 0.34 0.014 0.01 12.69 1.16 0.024 0.044 0.28 0.031 0.009
3 17.19 2.05 0.36 0.025 0.01 12.38 1.81 0.014 0.051 0.23 0.029 0.007
4 16.88 2.09 0.41 0.015 0.01 12.92 1.25 0.022 0.04 0.41 0.028 0.005
5 17.4 2.11 0.5 0.01 0.01 12.37 1.07 0.018 0.018 0.22 0.026 0.007
6 17.03 2.11 0.41 0.016 0.01 13.05 1.31 0.024 0.041 0.26 0.031 0.005
7 17.54 2.26 0.49 0.012 0.01 12.42 1.09 0.022 0.011 0.23 0.03 0.006
δ-ferrite in an austenite matrix, or eq, Ni eq, and Cr eq/Ni eq were calculated for
microsegregation of alloying elements in the each heat.
dendritic weld microstructure. Welds were performed using a Hobart
The optimum 316L formulation must CT 150-DC autogenous welder. The welding
be weldable, and maintain as much corrosion was done in a glove box using a 3/32-in. diam.
resistance as possible after the material is thoriated tungsten electrode and a shield gas of
welded. With these issues in mind, the present 96% Ar-4% H2. The polarity was direct current
research was performed to identify the optimum electrode negative (DCEN), with a high current
AISI 316L compositions for use in welded of 86 amps and a maintenance current of 47
components in corrosive service. amps. Pulse frequency was 6 Hz, with a pulse
width of 50%. Weld speed was 2 rpm, or 6.3
Experimental Procedure in./min.
Weldability Study
The welds were visually examined and
Samples from seven heats of evaluated for presence of slag and cosmetic
commercially available 2.0 in. diam. AISI 316L appearance, and were ranked accordingly. A
electropolished tubing, with Cr eq/Ni eq ratios Fischer Ferritscope was used to measure the
ranging from 1.38 to 1.68, were orbitally and maximum ferrite obtained in each weld.
autogenously welded using fixed weld
Corrosion Study
parameters. After welding, ferrite was measured,
and the welds were inspected for slag and Twenty-one heats of commercially
appearance. available AISI 316L electropolished tubing with
Cr eq/Ni eq varying from 1.2 to 1.8 and sizes
The compositions of the seven heats are
from 0.25 in. to 2.0 in. in diameter were
given in Table 2. These values were determined
examined. Samples from each tube lot were
versus traceable 316 SS standards, by X-ray
orbitally and autogenously welded with welding
fluorescence (Cr, Mn, Mo, Ni, Si), optical
parameters varied to achieve an acceptable weld,
emission spectroscopy (Nb, P, Ti, Cu), and high
as defined by weld bead thickness and
temperature combustion/inert gas fusion (C, S,
appearance. After welding, ferrite was
N). Once the compositions were known, the Cr
WELDABILITY AND CORROSION STUDIES OF AISI 316L ELECTROPOLISHED TUBING
by Sunniva R. Collins and Peter C. Williams
measured, and welded tube samples from each by X-ray fluorescence (Cr, Mn, Mo, Ni, Si),
lot were evaluated for corrosion resistance using optical emission spectroscopy (Nb, P, Ti, Cu),
a standard ASTM electrochemical (critical and high temperature combustion/inert gas
pitting temperature) test method. fusion (C, S, N). Once the compositions were
known, the Cr eq, Ni eq, and Cr eq/Ni eq were
The compositions of the twenty-one
calculated for each heat.
heats are given in Table 3, along with the tubing
sizes of each heat. These values were Table 4 shows typical welding
determined versus traceable 316 SS standards, parameters for each of the five tubing sizes.
WELDABILITY AND CORROSION STUDIES OF AISI 316L ELECTROPOLISHED TUBING
by Sunniva R. Collins and Peter C. Williams
Table 4. Corrosion Testing: Typical Welding electrode set up was used consisting of the test
Parameters specimen, an SCE reference electrode inserted in
a Luggin probe, and two graphite rods as counter
Tube Current, Travel, Heat Joules/in. electrodes.
OD, in. amps in./min. input,
Joules Each welded specimen for CPT testing
was made by orbitally and autogenously welding
0.250 20 6.48 288 1334
two 4-in. long tubes. The welded specimens
0.375 21 5.87 439 1494
were cut so that the weld was 0.5 in. from one
0.500 29 5.43 842 2322 end, and the total length of each specimen was
1.000 42 4.36 3343 4244 2.0 in. All samples were masked to isolate the
2.000 39 3.38 8477 4974 test surface to the inner surface only. One end of
the tube was coated with a non-reactive lacquer
Welding parameters were allowed to change in to cover 0.06 in. of the ID, the face on the end of
order to achieve an acceptable weld. Specimens the tube, and 0.25 in. of the OD. The outside of
from each heat were fabricated from tube stubs the tubing was masked with Plater’s tape,
orbitally and autogenously welded using the leaving 0.25 in. uncovered at the unlacquered
Swagelok Weld System. The welding was end. Electrical contact was made here by
performed using ceriated tungsten electrodes and connecting a coated copper wire to the tubing
a shield gas of 100% Ar. with a hose clamp.
The electrochemical Critical Pitting Approximately one inch of the specimen
Temperature (CPT) test (based on ASTM G was submerged vertically in the solution, with
150) (16) to determine resistance to localized the weld 0.5 in. from the submerged tube end,
(pitting) corrosion was performed. The CPT test and equilibrated for 10 min. at 0 °C. Following
measures the temperature at which current the initial delay, a potential of 700 mVSCE was
density increases rapidly beyond a set limit at a applied to the sample while the temperature was
set electrical potential. A NaCl solution is used, raised one degree (°C) per minute. Due to a
and the electrical potential is held constant in the delay in heating, this rate was not actually
passive region. Starting at a temperature of 0°C, realized until 10 °C. Current was measured
the temperature is raised slowly at a rate of 1°C continuously. The test was ended when the
per minute until pitting occurs. current density exceeded 100 µA/cm2 for 60 s,
The test solution was 3.56% NaCl made which signified the onset of localized corrosion.
from reagent grade chemicals and DI (17 MΩ) The specimen was then removed from the cell
water. A temperature controller was employed, and rinsed in DI water. All specimens were
with its probe inserted so that the tip was examined to identify the location of the pitting
touching the test specimen. A glass cooling coil and to inspect for under-lacquer corrosion.
circled the inside wall of the beaker. A chiller Specimens that showed signs of under-lacquer
pumped coolant through the glass coil to provide corrosion were discarded. At least six valid
cooling. Heating was provided by a heating repetitions were performed for each heat.
mantle sized to fit snugly around the beaker. An The method used differed from ASTM
immersible magnetic stirring plate and bar at the G 150 in that a stir bar was used in place of
bottom of the beaker was used to reduce nitrogen gas for agitation. Additionally, several
temperature gradients in the cell. The test cell data points that were <10 °C, were reported as
was a 2 L glass beaker cut to 4.5 in. high and their exact value, not as <10 °C as indicated in
capped with a polyethylene cover. A three- the standard.
WELDABILITY AND CORROSION STUDIES OF AISI 316L ELECTROPOLISHED TUBING
by Sunniva R. Collins and Peter C. Williams
4
3 Heat Ni eq Cr eq Cr % CPT,
2 No. eq/Ni Ferrite, ºC,
1 eq max avg
0
8 14.03 21.63 1.54 2.24 22.6
1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75
Cr eq/Ni eq 9 12.71 21.12 1.66 3.58 16.3
10 13.62 20.28 1.49 2.23 13.1
Figure 4 % Ferrite vs Cr eq/Ni eq
11 16.02 21.78 1.36 0.23 23.1
Prior to corrosion testing, a Fischer 12 13.59 20.90 1.54 1.73 16.4
Ferritscope was used to measure the maximum
% ferrite obtained in each weld. After corrosion 13 13.97 21.45 1.54 2.39 23.9
testing was completed, the CPT results were 14 13.57 20.51 1.51 1.62 22.3
compared to % ferrite and Cr eq/Ni eq.
15 13.26 21.24 1.60 3.87 20.4
Results and Discussion
16 13.92 21.00 1.51 1.81 12.4
The Cr eq/Ni eq ratio of Hammar and
Svensson appears to be an excellent predictor of 17 13.59 20.09 1.48 0.70 10.2
ferrite formation in autogenously welded 316L. 18 12.26 20.27 1.65 4.53 4.1
Figure 4 shows maximum measured % ferrite
versus Cr eq/Ni eq for the twenty-eight heats in 19 12.71 21.05 1.66 5.15 15.5
both the weldability and corrosion studies. It is 20 14.05 20.99 1.49 1.36 13.9
Table 5. Weldability Testing: Calculated 21 16.11 21.78 1.35 0.21 20.6
Values of Ni eq, Cr eq, and Cr eq/Ni eq; and
22 15.93 21.81 1.37 0.29 20.1
Measured Maximum % Ferrite in Welds
23 15.68 21.91 1.40 0.30 18.2
Heat No. Ni eq Cr eq Cr eq/Ni eq %
24 12.23 20.72 1.69 6.40 7.0
Ferrite,
max 25 13.63 20.67 1.52 2.38 12.3
1 12.09 20.33 1.68 3.91 26 13.85 20.51 1.48 1.21 10.6
2 14.48 20.31 1.40 0.27 27 13.16 20.37 1.55 3.23 13.2
3 14.20 20.62 1.45 0.82 28 13.61 21.14 1.55 3.93 15.9
4 14.77 20.42 1.38 0.00
5 13.57 21.09 1.55 2.07 interesting to note that both sets of data are well
predicted by Cr eq/Ni eq, despite differences in
6 14.83 20.60 1.39 0.15 weld setup (different shielding gases, part
7 13.63 21.43 1.57 3.04 rotation versus weld head rotation, different
rotational speeds, etc.).
WELDABILITY AND CORROSION STUDIES OF AISI 316L ELECTROPOLISHED TUBING
by Sunniva R. Collins and Peter C. Williams
Figure 5 Visual appearance of welds in 2.0 in. diam. 316L tubing arranged according to Cr eq/Ni eq
From left: Heat 4 (1.38); Heat 6 (1.39); Heat 2 (1.40); Heat 3 (1.45); Heat 5 (1.55); Heat 7 (1.57); Heat 1 (1.68).
20 slope = -0.77
15
Corrosion Study
10
slope = -2.74
5
Table 6 lists the calculated values of Cr
0
eq, Ni eq, and Cr eq/Ni eq, and measured
0 1 2 3 4 5 6 7 maximum % ferrite and CPT, for Heats 8
% Ferrite
through 28. Figure 6 shows CPT versus
maximum % ferrite. Figure 7 shows CPT versus
Figure 6 Critical Pitting Temperature vs % Cr eq/Ni eq. The corrosion resistance of welded
Ferrite 316L as measured by CPT falls off dramatically
when % ferrite in the weld exceeds 3% max.
30
This effect can be seen by comparing the slope
25
of the linearized data for ferrite contents below
CPT, degree C
20 slope = -20.9
and above 3%. Above 3% ferrite, the CPT drops
15
off approximately 3.5 times as fast as below 3%
10 slope = -67.2
ferrite. This same break point occurs when Cr
5 eq/Ni eq exceeds 1.55. The drop off in CPT with
0 increasing ferrite content (and increasing Cr
1.35 1.40 1.45 1.50 1.55 1.60 1.65 1.70 1.75
eq/Ni eq) is also noted by the shift downward of
Cr eq/Ni eq the range of the data, as indicated by the dashed
lines.
Figure 7 Critical Pitting Temperature vs Cr eq/Ni eq Conclusions
• Slag forming elements, such as Al, Ca, Si,
Weldability Study Zr, or Ti, have a higher maximum solubility
Table 5 lists the calculated values of Cr in bcc ferrite than in fcc austenite.
eq, Ni eq, and Cr eq/Ni eq, and measured Therefore, a 316L composition that
maximum % ferrite, for Heats 1 through 7. solidifies in the ferritic-austenitic mode will
Figure 5 shows photographs of welds from show a greatly decreased propensity for the
Heats 1 through 7, arranged according to Cr formation of slag on the weld.
eq/Ni eq. From visual inspection, a change in the
morphology of the weld is noted at
WELDABILITY AND CORROSION STUDIES OF AISI 316L ELECTROPOLISHED TUBING
by Sunniva R. Collins and Peter C. Williams
13. A. Garner, “The Effect of Autogenous 15. N. Suutala and M. Kurkela, “Localized
Welding on Chloride Pitting Corrosion in Corrosion Resistance of High Alloy Austenitic
Austenitic Stainless Steels,” Corrosion, Vol. 35, Stainless Steels and Welds,” Proc. Conf.
Mar. 1979, pp. 108-114. Stainless Steels ‘84, Goteberg, 3-4 Sept. 1984;
Institute of Metals, London, 1985, pp. 240-247.
14. P. I. Marshall and T. G. Gootch, “Effect
of Composition on Corrosion Resistance of 16. ASTM G 150, “Standard Test Method
High-Alloy Austenitic Stainless Steel Weld for Electrochemical Critical Pitting Temperature
Metals,” Corrosion, Vol. 49, June 1993, pp. 514- Testing of Stainless Steel,” in Annual Book of
526. ASTM Standards, ASTM, West Conshohonken,
PA, 1998.