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Proceedings of the ASME 2017 Pressure Vessels and Piping Conference

PVP2017
July 16-20, 2017, Waikoloa, Hawaii, USA

PVP2017-65801

IMPACT TOUGHNESS DEFICIENCIES IN ASME SA-350 LF2 FLANGES

R. M. Thompson K. C. Baker
Chevron Energy Technology Company Chevron Energy Technology Company
Houston, TX, USA Houston, TX, USA

ABSTRACT forensic laboratory for investigation. While the defects were


Personnel working on a major capital project experienced a found to be superficial in nature, mechanical testing of samples
significant issue related to the supply of non-conforming removed from the flanges revealed non-conforming impact
ASME SA-350 LF2 low temperature carbon steel (LTCS) weld strength, yield strength, and/or tensile strength. The values
neck flanges. Flanges were destructively tested and found to were far below the acceptance criteria in the SA-350
have Charpy impact toughness far below minimum values specification, and did not match the values on the material test
required by the ASME specification. The scope of this issue certificates. At this point, additional testing and detailed
involved several thousand flanges, and the nature of this non- investigation of manufacturing records was initiated, which
conformance could have resulted in the unexpected failure revealed a widespread and systemic problem with these heat
while in service. In all cases, mill certificates supplied for the exchanger flanges. Despite the fact that the documentation was
flanges did not indicate any deviation from the ASME all in conformance with requirements, the mechanical
specifications. The investigation revealed that industry properties were often found to be deficient when testing
standards are not adequate to identify and prevent this potential samples removed from the actual flanges. Attempts were made
problem, therefore highlighting the need for changes to be to sort flanges by non-destructive means such as hardness
made. This paper details the experience and investigation, and testing and portable chemical analysis, but these methods of
includes suggestions for improvement to the ASME assessment were not successful in identifying non-conforming
specification. flanges. Ultimately, the decision was made to reject all of the
subject flanges, cut them from the equipment, and replace with
INTRODUCTION material from a different supplier.
A large number of carbon steel air cooled heat exchangers were
required for a recent major capital project. These exchangers BACKGROUND
were designed to a minimum temperature of -46°C (-50°F), and ASME SA-350 LF2 is a commonly used carbon steel flange
therefore required the use of impact tested material. The specification when impact testing is required for design
equipment order was placed with a single manufacturer, who conditions. The specification has typical carbon steel
then subcontracted supply of individual components to various chemistry requirements, minimum required mechanical
sub-suppliers, which included two flange manufacturers using properties, and a mandatory heat treatment for forgings used to
three different raw material suppliers. The material was make ASME B16.5 flanges, which is most commonly
specified in accordance with ASME SA-350 LF2 [1]. Almost normalizing. The chemical composition requirements are
3000 ASME B16.5 [2] flanges were supplied ranging in size shown in Table 1. Mechanical property requirements are listed
from DN50 to DN300 (2 inch to 12 inch) and pressure ratings in Table 2.
from Class 150 to 1500. These flanges were then used for heat
exchanger manufacturing, welded into header boxes as For mechanical testing purposes and for forgings that are less
required, tested per all requirements, and delivered to the than 4536 kg (10,000 lbs), the manufacturer is permitted to use
project. a separately forged test block that is intended to represent the
finished product. The size of this test block is required to be
During routine visual inspection, some damage was observed 100mm (4 inches) x 100mm (4 inches) x T, where T can be no
on a few flange faces. These flanges were cut off and sent to a less than 6mm (1/4 inch) smaller than the thickness of the parts

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which it represents. The standard test location is 1/2T for precipitates, such as titanium, niobium (columbium), or
thickness less than or equal to 50mm (2 inches) and 1/4T for vanadium. Of note should be the fact that ASME SA-350 does
thickness greater than 2 inches (50mm). Subject to furnace not require any specific method of fine grain practice, nor is
control requirements, only one tension test and one set of 3 there any requirement for verification testing to prove
impact tests is needed per heat, and not every heat treat lot effectiveness. There are no minimum values for any of the
needs to be tested. elements that are known to produce fine grain practice, and no
reporting requirements for the more commonly used aluminum
and nitrogen.
Table 1: Chemical requirements (wt. pct.) as specified by
ASTM A350 LF2. INITIAL TESTING
C Mn Si Ni Cr Mo Ti Including the testing of the first set of defective flanges, a total
0.30 0.60-1.35 0.15-0.30 0.40 0.30 0.12 N/R of 58 flanges were selected for destructive examination
representing 5 different heats of material in the supply scope.
Nb V Al N S P Cu Sizes ranged from DN50 to DN300 with the most commonly
0.02 0.08 N/R N/R 0.040 0.035 0.40
tested being DN150 and DN250 (40 of 58). Pressure rating
N/R = Reporting is not required
Single values are maximums ranged from Class 150 to 1500 with most of those tested being
Class 300 and 600 (46 of 58). All of the flanges were subjected
to chemical analysis, tensile testing, and charpy impact testing.
Table 2: Mechanical property requirements as specified by Mechanical testing was performed in both axial and tangential
ASTM A350 LF2 Class 1. orientation where flange size permitted (about half of those
Yield Tensile Impact toughness, J Impact toughness, J (ft- tested) with samples extracted from locations specified in DNV
Strength, Strength, (ft-lbs) lbs, minimum single value OS-F101 [6]. All mechanical testing was performed in
MPa (ksi) MPa (ksi) Average of 3 at -46°C at -46°C (-50°F) accordance with ASTM A370 [7] using the largest sample size
(-50°F)
250 (36) 485-655 20 (15) 16 (12)
possible. Chemical analysis was performed using atomic
(70-95) emission spectroscopy (AES).

RESULTS
Fine Grain Practice Of the 58 flanges tested, 49 failed to meet the impact testing
Like many other carbon steel specifications, ASME SA-350 requirement of 20J (15 ft-lbs) minimum average of 3 specimens
requires the use of fine grain practice in order to improve with many also failing tensile test requirements (results below
toughness properties. A common method of fine grain practice minimum required yield or tensile strength (UTS) or both).
is by the use of aluminum and nitrogen additions to the steel to Thirty-one flanges had toughness of 5J (3.7 ft-lbs) or less when
form Aluminum Nitride (AlN) precipitates at the grain tested at -46°C (-50°F). There were some differences in results
boundaries, which help prevent grain growth during for transverse and axial orientation, but in almost all cases, both
manufacturing operations such as forging and heat treatment. orientations passed or both orientations failed for any one item
This practice is very effective at maintaining the grain size of a where both orientations were tested. Failures were seen in all
forging as long as the temperature is not increased to the point five heats that were tested.
that the AlN dissolve and go back into solution. Once in
solution, there are no precipitates pinning the grain boundaries Chemical analysis results were examined for the failed items
which leads to rapid coarsening of the grains and a degradation and in particular, the Mn/C ratio was compared with impact test
of the low temperature Charpy toughness. values. Figure 1 presents the results where each of the impact
test values is the average of three tangential samples for a
Some industry specifications have defined requirements for single flange.
aluminum and/or nitrogen that would be required to achieve
fine grain practice. For example, ASME SA-6 [3] requires a
minimum of 0.02% total aluminum for a steel to be considered
fine grain without a grain size test. Aluminum to nitrogen ratio
is also important to ensure there enough free aluminum to react
with the nitrogen and that there is not an excess of nitrogen,
which has been shown to increase the ductile-to-brittle
transition temperature [4]. Some specifications such as EN
10225 [5] suggest a minimum aluminum to nitrogen ratio of 2.

Other less-common methods of fine grain practice involve


small additions of other elements to form grain-pinning

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of the four flanges. In addition, the average prior austenite
grain (PAG) size upon reheating was also determined using the
McQuain Ehn method. The grain size was estimated per
ASTM E112-13 “Standard Test Methods for Determining
Average Grain Size” [9].

Seven Vickers hardness measurements (HV10) were acquired


for each metallographic mount in the as-polished condition.
The hardness measurements were subsequently converted to
Rockwell B hardness per ASTM E140-07 [10].

Table 4: Chemical composition (wt. pct.) from AES and


combustion analysis.
Figure 1: Mn/C ratio vs. Charpy V-notch impact toughness for
all 58 flanges tested. Flange C Mn Si Ni Cr Mo Ti
1 0.16 1.31 0.29 0.011 0.026 0.002 0.001
2 0.17 0.94 0.17 0.007 0.016 0.001 0.001
3 0.20 0.91 0.20 0.004 0.010 0.001 0.002
4 0.20 1.17 0.26 0.009 0.017 0.001 0.001
MORE DETAILED EXAMINATION
Four of the tested flanges were identified for further analysis. Flange Nb V Al N S P Cu
These flanges were all supplied by a single forge shop but the [ppm]
steel was sourced from multiple suppliers. These four flanges 1 0.02 0.034 0.034 60 0.006 0.014 0.023
were identified for further analysis because they spanned a 2 0.001 0.001 0.033 80 0.007 0.010 0.009
range of toughness from 3 to almost 200 J (2.2 to 147 ft-lbs) at 3 0.001 0.002 0.006 90 0.009 0.018 0.003
4 0.001 0.001 0.032 60 0.005 0.008 0.009
-46°C (-50°F) with nominally the same chemical composition.
The flange size and heat treatment for each of the four flanges
Table 5: Carbon equivalent (CE) and the ratio of Mn/C and
are shown in Table 3.
Al/N for each of the four flanges analyzed.
The chemical composition of the four flanges as determined by
AES and combustion analysis (N only) are shown in Table 4. Flange CE IIW Mn/C Al/N
The carbon equivalent (CE) per the International Institute of 1 0.39 8.4 5.7
Welding (Eq. 1) [8] and the Mn/C and Al/N ratio are shown for 2 0.33 5.5 4.1
reference in Table 5. 3 0.35 4.6 0.7
4 0.40 5.8 5.3
CE = C + Mn/6 + (Cr+Mo+V)/5 + (Cu+Ni)/15 Eq. 1
RESULTS FROM MORE DETAILED TESTING
Charpy V-Notch Testing
Table 3: Flange size and post-forging heat treatment as
The Charpy V-Notch results for axial and tangential testing at -
reported on the MTR for the four flanges analyzed.
50°F (-46°C) as well as the reported impact energy from the
material test report (MTR) are shown in Figure 2. Flange 1
Flange Heat Treatment
(169.5 ± 31.2 J), exhibited the highest overall impact energy
Size, Temp., °C Duration, Cooling followed by Flange 4 (109.8 ± 9.5 J), Flange 2 (32.5 ± 13.6 J),
mm (in) (°F) hours Type and finally Flange 3 (4 ± 0 J). The axial orientation resulted in
Flange 1 152.4 (6) 900 (1652) 6.5 Air Cool lower toughness values for all flanges except Flange 2 and
Flange 2 254 (10) 890 (1634) 8 Air Cool there was also generally more scatter observed in the axial than
Flange 3 152.4 (6) 900 (1652) 6.5 Air Cool tangential data. It should be noted that none of the test results
Flange 4 254 (10) 1070 (1598) 6.5 Air Cool were consistent with the reported MTR values for any of the
four flanges destructively tested.
Microstructure and Hardness Characterization
To help in understanding the differences in toughness, Mechanical Property Determination
metallographic samples were examined in the as-polished and The mechanical property results (yield strength and ultimate
etched (2 pct. Nital) conditions. Metallographic samples were tensile strength) in the axial and tangential orientations for the
made from the axial hub locations of the flanges. The general four flanges are shown in Figure 3. Even though a large range
microstructure and phase percent of each microstructural of impact energy values were observed for the four flanges, the
constituent (i.e. ferrite and pearlite) were determined for each yield and ultimate tensile strength are relatively consistent

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between the four flanges and the two orientations. All four
flanges met the yield strength specification while only three of
the four flanges met the ultimate tensile strength requirement of
ASTM A350 LF2. Flange 2 met the yield strength requirement
but did not meet the minimum ultimate tensile strength of 482
MPa (70 ksi) instead only reaching 462 MPa (67.0 ksi) in the
axial orientation and 457 MPa (66.3 ksi) in the tangential
orientation.

Hardness Characterization
To aid in determining if there were differences in the
microstructure between the four flanges, hardness testing was
conducted. The average hardness with standard deviations for
each samples are shown in Figure 4. Even though a total of
seven indents were obtained for each of the four flanges, the
hardness measurements themselves were very consistent. The
small amount of scatter in the hardness data is indicative of Figure 2: Charpy V-notch impact values at -50°F for the four
normalized steels that have been air cooled. flanges in the axial and tangential orientations.

Microstructural Characterization
Microstructural characterization was undertaken for each of the
four flanges. The average grain size, phase fraction, prior
austenite grain size, and C content in wt. pct. are shown in
Table 6. All four flanges were composed of a ferrite/pearlite
microstructure with no martensite or bainite present. The
relative phase fractions for each of the four flanges are shown
graphically in Figure 5. Representative microstructural images
are shown in Annex A, Figures A1 to A4 while the prior
austenite grain size as revealed by the McQuain Ehn method
are shown in Figures A5 to A8.

Table 6: Quantitative microstructural characterization of the


four flanges examined.

Avg. Grain Size, Ferrite/ PAG size, Figure 3: Tensile properties (yield and ultimate tensile
ASTM (μm) Pearlite Pct. ASTM (μm) strength) for the four flanges in the axial and tangential
Flange 1 8 (22.5) 70/30 8.5 (18.9) orientations.
Flange 2 8 (22.5) 65/35 8 (22.5)
Flange 3 6 (44.9) 65/35 4.5 (75.5)
Flange 4 7.5 (26.7) 55/45 8.5[A] (18.9)
[A] Bi-modal grain size

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Figure 4: Microhardness testing converted to Rockwell B for Flange 1 was found to be a low carbon (0.16 wt. pct.) forging
the four flanges. Each bar represents the average of seven with a high Mn/C ratio (8.4) and microalloy additions of Nb
indents with the error bars showing the standard deviation. (0.02 wt. pct.) and V (0.034 wt. pct.). This flange exhibited
excellent low temperature toughness of 169.5 ± 31.1 J (125 ±
23 ft-lbs), Figure 2, and material strength that was within
specifications, Figure 3. The microstructure consisted of
mostly ferrite (70%) with smaller islands of pearlite (30%).
The distribution of ferrite and pearlite in the microstructure was
relatively even, and the ferrite and pearlite grain size were also
consistent throughout the alloy. The prior austenite grain size
(ASTM number 8.5) was also consistent throughout the alloy
and of the same size as the resulting room temperature
ferrite/pearlite microstructure (ASTM Number 8). The fine
prior austenite grain size and ferrite/pearlite microstructure
indicated that the aluminum and nitrogen additions were
sufficient to form AlN at the grain boundaries that resisted
grain coarsening during the normalizing heat treatment.

Though the ferrite mean free path (i.e. continuous network of


ferrite grains) was relatively large in this alloy the microalloy
Figure 5: Phase percent of pearlite and ferrite in each of the addition of Nb and V were effective at strengthening the ferrite
four flanges at the axial hub. phase which is evidenced by the materials strength
characteristics (yield and ultimate tensile strength). This
DISCUSSION material had a very similar microstructure to Flange 2 but met
General Results all mechanical requirements due to the microalloy addition.
The high number of non-conforming flanges is clearly of Even though microalloy additions can increase the ductile to
significant concern especially given that the material brittle transition temperature, the low strength ferrite/pearlite
certificates had all indicated good quality material. While microstructure resulted in little if any increases [13].
detailed assessment was not performed for all 58 flanges tested,
some conclusions may be drawn from the information Results of more detailed testing - Flange 2
collected. In particular, a strong correlation was observed Flange 2 was found to be a low carbon (0.17 wt. pct.) and low
when comparing impact toughness testing results to manganese Carbon Equivalent (CE=0.33) forging with a moderate Mn/C
to carbon ratio (Mn/C), Figure 1. This observation has also ratio (5.5). This flange exhibited acceptable but lower
been made by other researchers, and this parameter has long toughness of 32.5 ± 13.6 J (24 ± 10 ft-lbs), Figure 2, and
been known as a general indicator of expected toughness for tensile strength lower than the minimum specification,
carbon steel components [4,11,12]. It has been found that Figure 3. There was more ferrite (65%) than pearlite (35%)
increasing Mn/C ratio results in decreasing transition which is consistent with the carbon content of this alloy. The
temperature, a tighter transition temperature range, and an grain size (ASTM number 8) was consistent with Flange 1 but
increase in the maximum toughness [4]. the prior austenite grain size (ASTM number 8) was slightly
larger than Flange 1. However, the low temperature toughness
The effect of manganese itself is also known to be beneficial. and tensile strength were much lower than Flange 1. The
Increases in manganese reduce grain size, allow greater discrepancy in properties was mostly due to the lower
spheroidization of carbides, decreases amounts of cementite manganese content which accounted for most of the difference
film around pearlite grains, and increases solubility of carbon in CE compared with Flange 1 – CE 0.39 vs. CE 0.33. The
in ferrite. All of these effects can help increase impact microstructure of Flange 1 and 2 were very consistent between
toughness [4]. each other but with lower Mn content, and without the
microalloy addition, the ferrite phase was not strengthened
While the test results here support a Mn/C ratio minimum, which reduced the strength characteristics of the alloy.
determining a recommended value for ASME A350 LF2 Additionally, the microalloy addition combined with a slightly
material may require more work. Clearly Mn/C less than 6 is finer prior austenite grain size in Flange 1, ASTM number 8
an indicator of poor toughness, but no material was tested in versus 8.5, which led to the improved low temperature
the range of 6-8 making it difficult to select an appropriate toughness values as opposed to Flange 2.
minimum value.
Based on the chemical composition and microstructure of this
Results of more detailed testing - Flange 1 alloy, it can be concluded that higher Mn content and higher

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CE, and possibly small microalloy additions of Nb, V, and Al  Aluminum additions are important to help maintain a
would have improved the material strength and low fine grain size and to tie up free nitrogen that can
temperature impact energy values. Alternately, a faster cooling increase the ductile to brittle transition temperature.
rate than a still air cool (i.e. forced air cool) would have Nitrogen must also be present to allow formation of
resulted in a finer microstructure which would have improved AlN precipitates, which pin the grain boundaries.
both the material strength and low temperature impact energy  Material strength characteristics (yield and ultimate
values. tensile strength) are not good indications of low
temperature toughness performance. All four flanges
Results of more detailed testing - Flange 3 subjected to more thorough testing had similar yield
Flange 3 was found to be a low carbon (0.20 wt. pct.) forging and ultimate tensile strengths but very different low
with a low CE (0.35), low Mn content, low Mn/C ratio (4.6), temperature toughness performance.
and no aluminum addition. This flange exhibited very poor
low temperature toughness of 4 ± 0 J (3 ± 0 ft-lbs), Figure 2, RECOMMENDED CHANGES TO SPECIFICATIONS
and material strength that was within specification, Figure 3. As a result of this experience, several improvements to the
There was more ferrite (65%) than pearlite (35%) which is ASME SA-350 specification could be made to prevent a
consistent with the carbon content of this alloy. Without an reoccurrence and to limit the need for specific company
aluminum addition the grain size during forging and ordering requirements.
normalizing was not constrained which led to the larger grain  Methods of achieving and evaluating fine grain
size in the microstructure (ASTM number 6) and large prior practice are not presently covered in the standard.
austenite grain size (ASTM number 5). This coarse grain size While there are several means of achieving fine grain
resulted in the poor low temperature impact energy values. The practice, minimum aluminum and nitrogen content
amount of free nitrogen in this material, 90 ppm, also increased should be considered as a relatively inexpensive
the ductile to brittle transition temperature. Free nitrogen (not means of ensuring improved properties. Total
bound as precipitates) acts similarly to carbon by both aluminum greater than 0.02% would be one suggested
strengthening the steel and increasing the transition improvement with Al/N > 2.
temperature.  Heat treatment temperatures for normalizing are not
presently specified. More concise heat treatment
Results of more detailed testing - Flange 4 controls such as a normalizing temperature range may
Flange 4 was found to be a low carbon (0.20 wt. pct.) forging be needed to avoid dissolving grain refining
with a moderate Mn/C ratio (5.8). This flange exhibited good precipitates.
low temperature toughness of 109.3 ± 10 J (80.6 ± 7.4 ft-lbs)  A minimum required Mn/C ratio would be beneficial.
(Figure 2), and material strength that was within specification More work may be needed to define the optimal value,
(Figure 3). There was more ferrite (55%) than pearlite (45%) but this work would support a minimum ratio of 6.
which is the least consistent with the equilibrium ferrite and  Better testing procedures are needed to be sure the
pearlite content (25% ferrite and 75% pearlite). The average properties of the actual flanges more closely match the
grain size was found to be an ASTM number 8. The prior values reported on test certificates. Unless a
austenite grain size, however, was reported as an ASTM manufacture has correlation data to support using a
number 8.5 but examination of the micrograph reveals a bi- test blank, actual production forgings should be used
modal distribution of the grains, Figure A8. This bi-modal for testing purposes on a heat treat lot basis. Sizing
distribution was likely caused by normalizing at a temperature and pressure rating is also important, i.e. a DN150
high enough to dissolve the AlN present in the material to Class 300 forging cannot be used to qualify a much
prevent this type of grain coarsening. larger DN600 Class 900 item.
CONCLUSIONS ACKNOWLEDGEMENTS
From the metallurgical investigation coupled with the chemical The authors wish to acknowledge the significant technical
composition and mechanical testing the following conclusions contributions from Andrew Nissan [14].
can be made:
 The most effective method of improving low REFERENCES
temperature toughness is to refine the grain size of the [1] ASME Standard SA-350, “Standard Specification for
steel. The smaller the grains, the better the low Carbon and Low-Alloy Steel Forgings, Requiring Notch
temperature toughness. Toughness Testing for Piping Components,” ASME Boiler
 Lower carbon content and higher manganese content and Pressure Vessel Code, Section II-A, ASME, New
(high Mn/C ratios) clearly improve low temperature York, NY, USA, 2015.
Charpy impact toughness. A Mn/C ratio less than six
correlated with reduced low temperature toughness.

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[2] ASME B16.5-2013, “Pipe Flanges and Flanged Fittings”,
ASME, New York, NY, USA.
[3] ASME Standard SA-6, “Specification for General
Requirements for Rolled Structural Steel Bars, Plates,
Shapes, and Sheet Piling”, ASME Boiler and Pressure
Vessel Code, Section II-A, ASME, New York, NY, USA,
2015.
[4] M. Szczepański, The Brittleness of Steel, New York: John
Wiley and Sons, 1963.
[5] EN 10225:2009, “Weldable Structural Steels for Fixed
Offshore Structures – Technical Delivery Conditions”,
European Committee for Standardization, Brussels,
Belgium, June 2009.
[6] Offshore Standard DNV OS-F101, “Submarine Pipeline
Systems”, Det Norske Veritas, Oslo, Norway, October
2010.
[7] ASTM Standard A370-14, “Standard test methods and
definitions for mechanical testing of steel products”,
ASTM International, West Conshohocken, PA, USA.
[8] ASM Handbook, Vol. 6, Welding, Brazing, and Soldering,
ASM International, Materials Park, OH, 1993.
[9] ASTM Standard E112-13, “Standard Test Methods for
Determining Average Grain Size,” ASTM International,
West Conshohocken, PA, USA.
[10] ASTM Standard E140-07, “Standard Hardness Conversion
Tables for Metals,” ASTM International, West
Conshohocken, PA, USA.
[11] F. W. Boulger et al, “The Influence of Carbon and
Manganese on the Properties of Semikilled Hot Rolled
Steel,” Transactions of AIME, Vol. 6, No. 5 (1954), pp.
645-652.
[12] R. L. Sindelar et al, “Mechanical Properties For Fracture
Analysis of Mild Steel Storage Tanks”, US Department of
Energy, OSTI database.
[13] S. Shanmugam et al, “Impact Toughness and
Microstructure Relationship in Niobium- and Vanadium-
Microalloyed Steels Processed with Varied Cooling Rates
to Similar Yield Strength,” Materials Science and
Engineering A, Vol. 437, No. 2 (2006), pp. 436-445.
[14] A. B. Nissan et al, “Determination of the Cause of Low
Temperature Charpy Toughness Values in ASTM A350
LF2 Flanges”, Proceedings of the 28th ASM Heat Treating
Society Conference, October 20–22, 2015, Detroit,
Michigan, USA.

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ANNEX A

MICROSTRUCTURES OF FOUR FLANGES TESTED

(a) (b)
Figure A1: Flange 2 overall microstructure and (b) zoomed-in
image of the microstructure.


(a) (b)
Figure A2: Flange 2 overall microstructure and (b) zoomed-in
image of the microstructure.

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(a) (b)
Figure A3: Flange 3 (a) overall microstructure and (b)
zoomed-in image of the microstructure.


(a) (b)
Figure A4: Flange 4 (a) overall microstructure and (b)
zoomed-in image of the microstructure.

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Figure A5: Prior austenite grain etch of Flange 1 (revealed by Figure A7: Prior austenite grain etch of Flange 3 (revealed by
McQuain Ehn method) showing an equiaxed grain size McQuain Ehn method) showing very large equiaxed grains
throughout the sample. throughout the sample.


Figure A6: Prior austenite grain etch of Flange 2 (revealed by Figure A8: Prior austenite grain etch of Flange 4 (revealed by
McQuain Ehn method) showing an equiaxed grain size McQuain Ehn method) showing a bi-modal distribution of
throughout the sample. grain size which is indicative of a heat treatment that was
sufficiently hot to cause some of the AlN to dissolve and go
back into solution.

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