ANALYSISOFCRACKINGOFCO-EXTRUDED

RECOVERYBOILERFLOORTUBES
JR Keiser, B. Taljat, X.-L. Wang, R W. Swindetuan.,
P.J. Maziasz, RL. Thomas, and E.A. Payzant
Oak Ridge National Laboratory
Oak Ridge, Tennessee
D.L. Singbeil and R Prescott
Pulp and Paper ResearchInstitute of Canada
Vancouver, British Columbia

ABSTRACT
Cracking of the stainless steel layer in co-extruded
304USA2 10 tubing used in black liquor recoveryboilers is
being found in an ever-increasing number of North American
pulp and paper mills. Becauseof the possibility of a tube
failure, this is a signiticant safety issue, and becauseof the
extra time required for tube inspection and repair, this can
becomean economic issueas well.
In a project funded by the U.S. Department of Energy and
given wide support among paper companies,boiler
manufacturers, and tube fabricators, studies are being
conducted to determine the causeof the cracking and to
identify alternate materials and/or operating proceduresto
prevent tulx cracking. Examination of cracked tubeshas
permitted characterization of crack features, and transmission
electron microscopy is providing information aboutthe
thermal history, particularly cyclic thermal exposures,that
tubes have experienced. Neutron and x-ray diffraction
techniques are being usedto determine the residual stressesin
as-fabricatedtube panels and exposedtubes, and finite
element modeling is providing information about the stresses
the tubes experience during operation. Laboratory studiesare
being conducted to determine the susceptibility of the coextruded 304USA210 tubes to stresscorrosion cracking,
thermal &igue, and corrosion in molten smelt. This paper
presentsthe current statusof thesestudies.
On the basis of all of these studies, recommendationsfor
meansto prevent tube cracking will be offered,

Researchsponsoredby the U.S. Department of Energy,

Assistant Secretaryfor Energy Efficiency and Renewable
Energy, Offtce of Industrial Technologies, Advanced
Industrial Materials Program, under contract DR-ACOS96OR22464 with Lockheed Martin Energy ResearchCorp.

INTRODUCTION
Corrosion of water wall and floor
recovery
boilers representsa sign&ant hazard to the
?t!! e operationof
the boilers. Measurestaken to prevent, or control, corrosion
include the useof rigorous inspection and repair programs,
application of protective coatings to the surf& of tubes,and
the installation of co-extruded,or composite, tubeswith a
carbon steel core metallurgically bonded to a corrosion
resistant exterior layer. The use of axxtruded tubes,in
particular, has beenrecognized as solving many of the
corrosion problemsto which carbon steel tubes were prone,
and they have beenwidely specified for both new and retrofit
construction for the lower furnace walls and floors of kmft
recoveryboilers.
However, experiencegained from the use of co-extrudedtubes
in recoveryboiler servicehas also shown that they are subject
to someunique corrosion-relatedproblems. Rather than
general corrosion or thinning, the most common problem
affecting co-extrudedtubes in krafl recovery boilers has been
cracking which originates in the outer, stainless steellayer
(1). In many cases,the cracks are located close to, or
associatedwith, membraneor crotch plate welds at air port,
smelt spout and other openings in the boiler wall. Bare-face,
or crown cracking of tubes which form spout openings,floor
tubes,and portions of wall tubes exposedto the smeltbed is
also common, as is cracking along tube/membranewelds in
these latter locations, and in the membranesof tloor tubes.
In 1995, cracking of co-extruded tubes was identified as a
serious materials issuefacing the pulp and paper industry.
Consequently,a United StatesDepartment of Energy program
was establishedto determine the causeof the tubecracking
and to identify alternate materials or processchangesto
prevent this type of cracking. This project is being carried
out by researchersat the Oak Ridge National Laboratory
(ORNL), the Pulp and PaperResearchInstitute of Canada
(Paprican), and the institute of Paper Scienceand TechnoIogy
(PST) with strong support from more than a dozenpaper
companies,most major manufacturers of recoveryboilers, one
of the principal producersof co-extruded tubing, and
producers of other typesof tubing. The researchprogram
includes review of existing literature, microstructural
characterization of compositetubing, measurementof
residual stmssesin tubing, computer modeling to predict
stressesin compositetubesunder operating conditions, and
laboratory fatigue and corrosion tests. Collection and
analysesof operational data from mills, including tube
temperaturedata and chemical analysesof smelt, are also
being conducted. From this work it is expectedthat alternate
materials or operating procedureswill be identified that can
prevent cracking of compositetubes. This paper reportson
the current statusof this project.
a,

DISCLAIMER
This report was prepared as an account of work sponsored by an agency of the
United States Government. Neither the United States Government nor any agency
thereof, nor any of their employees, makes any warranty, express or implied, or
assumes any legal liability or responsibility for the accuracy, completeness,or uscftilness Of any information, apparatus, product, or process disclosed, or represents
that its use would not infringe privately owned rights. Reference herein to any spccific commercial prcduct, process, or service by trade name, trademark, manufacturer, or otherwise does not necessarily constitute or imply its endorsement, recommendation, or favoring by the United States Government or any agency thereof.
The views and opinions of authors expressed herein do not necessarily state or
reflect those of the United States Government or any agency thereof.

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BACKGROUND
General Information

A key issue in the researchprogram continues to be

identification of the mechanism of cracking. ~~gb
many
studies have been conducted with this intent, no clear
consensusabout the cracking mechanism yet exists. In m
this may be due to no single mechanism being responsiblefor
all of the observedcracking. The mechanisms most
frequently attributed with being the causeof this cracking
include thermal fatigue, stresscorrosion cracking (SCC), and
corrosion fatigue.
It is noteworthy that cracking of composite tubesis generally
limited to boiler floor tubes, wall tubes exposed to the smelt
bed, and tubes that form or are close to smelt spout openings
or air ports. Failure of unbent, vertical wall tubesis rare.
Where it has been reported, overheating (usually attributed to
excessiveinternal scaling) has been a significant contributor
to the failure. Mechanical constraints, in the form of welds to
crotch pIates and other attachments, clearly influence much of
the cracking which occurs at spout and air port openings.
Evidence has also been presented which suggeststhat cyclic
Wessesmay play an important role in cracking of smelt spout
opening tubes (1), but whether they are equally important for
cracking of floor tubes or for other unbent tubes is not clear.
Regardlessof the mechanism, cracking can only occur if
tensile stressesare present on the surface of the composite
tube. Due to the signi&zant difference between the thermal
expansion ccefficients of carbon steel and 304L stainless
steel, it has generally been assumedthat appreciabletensile
stresseswill exist in composite tubes. However, as will be
describedin the section on stressmeasurementsand
predictions, the stressstate in the stainless steel portion of a
compositetube is not n-y
easyto predict
Characteristic featuresof each of the proposed cracking
mechanismscan often be used to distinguish one from
another. Thermal fatigue occurs as a result of cyclic stresses
which are generatedby repeatedthetmal cycles. The stresses
generatedhave to reach the yield strength of the material,
which means,for the 304L stainless steel/carbon steelcoextruded tubes operating at 3OOC,the maximum
temperaturehas to reach at least 450C. In addition to the
requirement of a tensile stress, SW requires an appropriate
corrodent For stainlesssteels lie 304L, this could be a
concentratedalkaline environment at temperaturesin the
120-4OOCrange, or an aqueouschloride solution in the
temperatum range of 60-200C. In addition, sensitized
stainless steels are vulnerable to cracking when chromium
depletedregions adjacentto chromium carbide grain
boundary precipitates are exposed to polythionic acid. This

acid forms when a sulfide scale is cooled to room temperature

and exposedto moist air. A combination of bOrneof these
mechanisms,known as corrosion fatigue, can occur when a
combination of a corrodent and cyclic stressesare imposedon
a vulnerable material.
Mill Information
As the project hasprogressed a number of anecdotal
observationsaboutthe operation of recoveryboilers, and the
influence on cracking of composite tubes hasbeencollected
One sign&ant observation is that the fireside surfacesof
floor tubesin a recovery boiler are subjectto thermal
fluctuations asa part of normal boiler operation (24). This
has beenconfhmed in a number of boilers by meansof
surface-mounted,or slightly sub-surfacemounted,
thermocoupleson membranesand floor tubes. Generally the
magnitudeof thesefluctuations is lessthan 5OC from the
nominal baselinetube temperature in the boiler, but
infrequently the increasescan be. 150 to 2OOC. Excursions
of as much as 45OC have been reported (5).
At least two Scandinavian boilers, one in Finland and one in
Sweden,are dry cleaned (6.7). This is understoodto mean
that either no water is allowed to come into contactwith the
floor tubes,or any water that is used is completely removedso
that the floor tubesdo not remain wet. Neither of these
boilers hasreportedcracking of the compositefloor tubes.
There is someindication that inspection of thesefloors has
not beenas thorough as is normally the casefor composite
tube floors in North American boilers. Nevertheless,this is
an intriguing observation, and strong efforts are being made
to obtain additional information. For comparison,cracking
was found in floor tubes of a North American boiler that had
been in servicefor about 18 months: During this operating
period the floor was not cleaned and inspected,but it was
water washedthree times (8).
The compositionof smelt has been well-documentedfor
processpurposes,but no direct association hasbeenmade
betweensmelt composition and floor tube cracking.
However,analysisof results reported by representativesof
Ahlstrom Machinery Corporation suggeststhat the smelt
immediately adjacentto floor tubes has a compositionthat is
significantly different from the bulk composition (9). The
smelt sampleshad a very thin layer adjacentto the floor tubes
in which the potassiumand sulfur contents were unusually
high. As part of this program, efforts are being madeto
collect samplesunder similar conditions and from a similar
location to determine if comparable results can be found for
other mills.
In the balanceof this paper, the results of researchwhich has
been principally conducted during the past year will be

reported. The significance of this work toward understanding

cracking of compositetubeswill be described,and the efforts
directed at identification of possible alternative materials or
operating procedureswill be discussed
RESULTS

Microstructural Studiesof CompositeTubes

A large number of cracked compositetubesfrom boiler
manufacturers, inspection companies,and paper mills have
been carefully examined in order to define the characteristics
of the cracking (10). In somecaseslarge panels have been
supplied when all or sign&ant portions of a floor have been
replaced, while others have come from floors in which single
tubes, or no more than a pair of adjacenttubes, have been
removed for examination. In addition to cracked tubes,
unexposedtubes supplied by four different tube fabricators,
have been included in the characterization studies. A number
of techniques have beenused to characterize the various tube
samplesincluding examination of standardpolished/etched
cross sections with light microscopesand scanning electron
microscopes,determination of elemental specieswith an
electron microprobe, evaluation of fine microstructural
features with a transmission electron microscope,and
hardnessmeasurementswith a microhardnesstester.
The typical crack in compositetubes originates at the outer
surface, is often much wider at that surface,has relatively
little branching in the portion of the crack near the tube
surface,and extends through much, if not all, of the stainless
steel layer (10). Crack branching may occur at mid-thickness
of the stainless steel layer. Cracks that go through the
stainless either end at the stainless steel/carbonsteel interface
or turn and proceedalong that interface. Vety few cracks
penetrate into the carbon steel basematerial, and thosethat
do are usually, but not always, associatedwith mechanical
constraints or crotch plate attachments(1). In many cases,
corrosion pits develop in the carbon steelwhen a crack tip
ends at the interface. Other than thesecorrosion pits, a few
isolated casesin which attack has proceededinto the carbon
steel have been found. In two of thesecases,the attack was
intergranular and could be traced only a few grains into the
carbon steel.
For many cracks, there is a strong indication that tensile
stmssesin the surface have openedthesecracks fairly
re0xnly; matching featuresor contours can be seenon both
sides of the crack (Fig. 1). In addition, careful *
metallographic examination of tube crosssectionscan often
reveal additional cracks which were not observedduring dye
penetrant testing, These cracks are generally quite short and
have not opened so that detection by dye penetrant is difficult.
Furthermore, these cracks are essentially always

transgranular and often have a limited amount of branch&

Examplesof suchcracks are shown in Fig. 2.
Samplestaken from tube sections from a number of boilers
have beenpreparedso that the samplecouldbe bent to expose
the fracture surfacesfor examination in an electron
microscope. Theseexposedsurfaceshavebeen studied to
determine if the characteristic markings of fatigue could be
identified but no such markings were found on any of the
samples.

Figure I Example of wide, transgranular crack with

matchingfeatures on each side of the crack in a co-extruded
304LBA210 compositetube.

Figure 2 Example of short, narrow, transgranular cracks

with somebranching in a co-extruded 304usA210 composite
tube.

Determination of Stresses
.

The importance of the surface stressstatein the proposed

cracking modeswas notedpreviouslyin this paper.

(bb
300 t

Consequently,a strong effort hasbeendirectedat

determinationof thesestressesthrough experimental
measurementsand finite element modeling.

Esperimental measurements.
Residual stressesmeasuredusing X-ray and neutron
diEaction in unexposed 304USA.210 coextruded tubing
from both major manufacturers have been reported (10).
These messeswere shown to vary significantly through the
wall of the tube, especially in the vicinity of the stainless
&&/carbon steel interface. For both suppliers, the axial and
tangential stresseswere compressiveon the outer surfaceof
the stainless steel. The surface stresseshad a cyclic pattern
aroundthe circumfkrence of the tube, and measurements
showed a similar pattern in the hardnessas measuredin the
axial direction along the surfaceof the tube. The cyclic nature
of the stmssesand the hardnessare most likely the result of
the final processing step, straightening, and the manner in
which the tube advancesthrough the straightener.
These measurementsshow that despite the variation in stress
values, as-fabricated 64 mm (2% inch) OD 304UCS tubesat
room temperature have compressiveaxial and hoop stresses
in the surface layers. For 76 mm (3 inch) OD 304LICS tubes,
the measuredresidual stressesshow greater variability, tensile
at somelocations and compressiveat others.
To determine if exposure in a recovery boiler has an intluence
on the residual stressesin composite tubes, tube panelswere
removed from operating nulls and analyzed with X-ray or
neutron difFraction. A two-tube section of 64 mm (2% inch)
OD 304UCS tubes was examined with X-ray diffraction to
determine the surf&e residual stresseson both sidesof the
section. To determine the through-thickness stressprofile, a
single-tube section of 3 inch OD 304L/SA210 composite
tubes was measuredwith neutron diffraction. Figure 3 shows
the surface residual stressesobtained by X-my diffraction at
the surface of the two-tube section, The fireside exhibits a
different residual stressstate than the cold side after service.
For both axial and hoop stresscomponents,the fireside
messeson the crown of the tube are tensile with a maximum
of 300 MPa, while the cold side stresseson the crown are
neutral or compressive. The through-thickness stressprofile
determined by neutron diffraction on the single-tube
specimenis shown in Fig. 4. Here, both the fireside and cold
side stressesare tensile after service; however, the fire-side
exhibits higher tensile residual stressesthan the cold side.
The maximum tensile stresson the surfaceis about 250 MPa.

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Figure 3 Hoop, u, and axial, a, surface residual stress

measuredon an exposedtwo-tube panel. Schematicsof the
specimensare shown on the side where the black dots
indicate locations of X-rq measurements.Theshadedareas
were not accessible to X-ray difiaction measurements
becauseof geometric constraints.
Theseexperimental results indicate that after exposureof the
tubesto service conditions, the residual stressesin the
compositetubes have becometensile on the fire-side at room
temperature.The marked difference in magnitudeof residual
stressbetweenthe fire and cold sidesof the tubesshowsthat
the tensile residual stresson the fire-side mustbe due to
Venice, rather than fabrication of the panels.
A number of alternative materials have beenproposedas
replacementsfor co-ex-truded304USA210 compositetubing.
One being tried in limited portions on boiler floors is Alloy
625 applied as a weld overlay on carbon steeltubes. The
through-thickness residual stressprofile in an as-welded
Alloy 62Ycarbon steel tube was evaluatedby neutron
diffraction, and results are shown in Fig. 5. Tensile stress
regions were found in the weld metal as well as in the heataffixted zone in the carbon steel. The maximum tensile stress
of 360 MPa, which is about 75% of the 0.2% yield strength of
the weld metal, was located in the weld overiay. The
experimentally determined residual stressprofile was
comparedwith the results of a finite elementanalysis

element modeling. This information is particularly important

when evaluating residual stresseswhich developin and
around the tube-to-membraneweld joint becausetheseare
especially detrimentalto the integrity and the service
behavior of the weldedpart. High tensile residual stmssesin
the region nearthe weld could promotefailure by any of the

postulatedmechanisms.
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Cold

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Figure 4 Through thickness residual stressprofile

determined by neutron diflraction in an exposedtube.
Residual stressesin the carbon steel on the cold side could
not be evaluated.
conducted in parallel with finite element modeling (FEM)
(11,12). It was found that the modeling results are in very
good agreementwith the experimental data, as is shown in
Fig. 5. Subsequently,a sim.ilarIy prepared weld overlay tube
was heat-treatedat 900C before the residual stresseswere
measured. It was found that the residual stressesoriginally
present as a result of tube fabrication had nearly vanished
(11).
The X-ray and neutron d.ifIiaction data provide very
important information about the room temperaturestressstate
of composite tubes,but measurementsunder the operating
conditions of a recovery boiler are not possible. However,
finite element modeling can use the measuredroom
temperature stressesand predict what would exist at
operating conditions. Such modeling has been usedto predict
the stressesat operating conditions as well as to determinethe
effect of various thermal cycles on stresses.

Finite element modeling.

Each step in the manufactureof a composite tube introduces
some stressesinto the material, from the initial extrusion to
welding through to installation in the-boiler as part of a wall
or floor panel. The contribution of each step in the
manufacturing processon the development of residual
stressesin the final fabrication can be calculated by finite

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Figure 5 Through-thicknessresidual stressprofile in a weld

overlay tube. Ehedashedlines are calculations from a finite
element analysis. (a) Axial stress, a, (b) Hoop stress,uee
and (c) Radial stress,a,
The first considerationin the finite element (FE) analysisto
be addressedwasthe tube-membraneweld cross-section.
Welding simulationwas performed such that the weld on one
side of the membranewns made first, the tube was cooled to
room temperature,then the weld on the other side was made.
The analysiswasperformed for the 304USA2 10 composite
tube with Type 312 stainless steel weld material. The stresses
that result from welding during panel fabrication along with
the stmsseswhich develop at service conditions becauseof
internal pressurktion and elevated operating temperatures
were subsequentlyusedin the three dimensional modeling of
the floor tubes.
A FE modelfor thermal analysis of the smelt-tube-fluid
systemwasdevelopedto thoroughly determine the

temperaturedistribution in the circumferential and radial

directions of the tube at normal operating conditions and
during temperatureexcursions. A relatively severe
temperatureexcursion on a small segmentof the tube surface,
measuredby a thermocouple (TC) positioned on the crown of
the tube and representedin Fig. 6, was used to estimatethe
tube temperatureexpectedduring one of thesethermal
excursions. It was assumedthat the temperature measuredby
the TC correspondsto the smelt temperature3.2 mm (l/8 in.)
from the tube surface, which is higher than the tube surface
temperature. The temperatureat the tube surfacewas
calculated basedon the assumptionthat the molten smeft is at
800C and temperature decreasedlinearly through the
solidified smelt layer. The time dependenttemperature
distribution was used in the 3D model along with the residual
stressesfrom manufacturing and the in-service loading to
analyze the stressstate during and after the temperature
excursions.

from manufacturing. Plastic deformation in the stainlesssteel

layer is not significant.
Since the modelpredicteda transition from compressive
surfacestresseson the tubes at operating temperaturesto
tensile stressesat ambient temperatures, thermo-mechanical
analysis of the cooling transient was then performed to
determine the temperatureat which the transition occurs. It
was assumedthat linear variations of temperature and
internal pressurizationoccmred with time (temperature
variation from 315 to 20C and pressurevariation from 8.6 to
0 MPa in 300 minutes. As shown in Fig. 8, the stressesat the
surfaceof the 304L SSlayer becometensile when the
temperaturedropsto 270 C and the material reachesits yield
stresswhen the temperaturereachesapproximately 220C.
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Figure 6 Typical temperature excursion measuredby afloor

thermocouple.
In order to define the stressand strain statesin a composite
tube as the result of operation, three dif&ent temperature
cycles were used:
- heating to operating temperatureand back to rmrn
temperature - two cycles,
- two consecutive appearancesof hot spotsat the
samelocation, and
- steamblanketing during the hot spot appearance.

Figures 7-10 show the temperaturevariation and the

corresponding hoop and axial stresscomponentsof the tube
crow-non the fireside surfacefor thesedifferent cycles. The
results for the first condition (cycling to a typical operating
temperature) show that the compressivestressesat operating
conditions exceedthe yield stressof the 304L SS layer, which
is around 100 h4Paat 300C. Surfacestresseson the crown
of the tube at room temperature after the first cycle are tensile
and considerably higher than the original residual stresses

0
0

200

400

640

8x

1000

ame 1s;

Figure 7 Temperatureand stressesfor case I

Mnnkaila

firesids
350

250

=I

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a
150

Figure 8 Temperatureand stressesduring cooIing transient.

The results for the secondcaseshow that the high

temperaturegradient through the tube thickness and the
them& expansion mismatch result in high stressesand
extensiveyielding in the 304L layer. Also, compressive
messesat the operating conditions exceedthe yield stress. A
temperatureexcursion causeshigher compressivestmssesand
comiderable yielding. Returning to operating conditions
causesstressreversal - high tensile stresseswhich exceedthe
yield stress. Stressesat normal operation after the
temperatureexcursion remain tensile at the location of the hot
spot. The secondtemperature excursion causesadditional
yielding which results in even higher tensile stresstier the
excursion. Cooling to rwm temperatureintroduces
additional yielding and raises the stresses,which are already
tensile beforecooling. A single temperatureexcursion can
producean equivalent plastic strain of about 1%, whereasthe
cumulative equivalent plastic strain at the location of multiple
temperatureexcursions can easily reach 2% or more.

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200

400
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600

800

Figure IO Temperatureand stresses for case 3.

Thermal Fatigue Evaluation of 304L Stainless Steel

2w

4w

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figure 9 Temperature and stressesfor case2.

The resuhs of the third caseshow that a higher tube
temperature,which is due to steamblanketing, causesa
pronouncedeffect of lateral constraint and thus larger
deformation and yielding of the carbon steellayer. The
presenceof steamblanketing causeshigher temperaturesat
the inside tube surface, which meansa smaller temperature
gradient through the tube thickness. The constraints provided
by adjacenttubes relieve the high compressivehoop stresses
and possibly causesmall tensile stressesat the fireside surface
during temperatureexcursions [instead of causing even
higher compressivestresses(case2)], which agreeswith
predictions of previous models (10). Stressesat the 304L
layer are tensile after the temperatureexcursion and remain
tensile during operation. Stressesin this caseare lower due
to the smaller temperature gradient through the tube
thickness.

Becauseof the significant difference in thermal expansion

coefficients of 304L stainless steel and carbon steel,there has
been speculationthat thermal fatigue might be responsiblefor
this cracking. Analytical, experimental, and metallurgical
studiesby Egnell and Tomblom (13) suggestedthat fatigue
cracking could occur for critical combinations of temperature
change, hold-time temperature, and cycles. They compared
their results against fatigue design cmves in the ASME Sect
III high temperaturecode case(now Sect.IlI, Div. 1, Subsect.
NH) and concluded that the useful life of the tubescould be
estimated from a theoretical stressanalysis and information
on the fatigue properties for the materials at the highest
temperatureof the thermal cycle. To further investigatethe
problem of floor tubes in recovery boilers, taskswere
undertaken to: (a) review fatigue in constituent alloys, (b)
produce data to assistin the analysis efforts, (c) fatigue test
tubes,and (d) determine cracking patterns for various
thermal/mechanical loadings for comparison with in-service
cracking characteristics.
The design cues in the ASME Code Sect.III, SubsectNH
were basedon isothermal testing of relatively coarse-grained
300 seriesH-grade stainless steels. Both mechanicaland
thermal fatigue data for 304H and 304L were colkcted for
comparison with the ASME design curves (14-N); and it was
observedthat the ASME design cmve for 427C is
conservativerelative to thermal fatigue data evenwhen the
maximum temperaturein the thermal fatigue cycle is well
above427C (seeFig. 11). Additional exploratory isothermal
testing of 304L stainless steel was undertakenfor comparison
to the design curve. A very fine-grained material (annealed

at 927C) was produced to simulate the cladding and tested

in fatigue at 600C with a 1% strain range and a 0.1 hour
hold time at the peak temperature. A sample failed at a life
longer than given by the design curve for 427C, as shown in
Fig. 12. A secondsamplewas cold 5orked 50% by rolling to
simulate the highest hardnessohservedin the cladding.
Under testing conditions similar to the annealed material, the
sample exhibited a fatigue life well beyond the ASME design
curve for 427C, as shown in the samefigure. A thermal
fatigue test was undertaken in which the specimenwas cycled
between
300C and 450C with a superimposedmechanical
strain to achieve 0.77% strain range. The specimen exceeded
3500 cycles without cracking. However, several issuesneed
to be resolvedbefore fatigue damagein the 304L stainless
steel cladding can be estimated These issuesconcern the
identikation of the peak temperature,the time sustainedat
the peak temperature,the strain accumulated in a cycle, and
the number of cycles.

I
0
10

100

1000
cyci*r

IO

10000

100000

fallurc

Figure 12 Comparisonoffatigue for fine-grained 304L

stainless steel with the ASME Sect. iii, Subsect.NH design
curvefor 304H stainless steels at 427 c (800 m.
design curves,the fatigue life would exceed 10,000cycles.
Actual fatigue data indicate a fatigue life beyond 100,ooO
cycles.

IO

100

10000

1000
Cycisr

to

100000

frifutc

metallurgical changescould be see5 afkr times as short as 24

hours. The coarsening of the carbide structure at the interface
was clearly visible in both cases(seeFig. 13). No such
carbide coarsening was observedin failed tubes,which
indicates that no significant times mereaccumulatedabove
480C. Ifit is assurnedthat rapid 300 to 450C transients
occur which are experiencedonly by the stainlesssteel, then
the maximum strain increment in the 304L stainlesssteel
cladding would not exceed0.3%. According to the ASME

The cracking of the fatigue specimenswas examinedfor

comparisonto the cracking patterns in exposedcladding.
Cracksproducedin the fine-grained 304L stainlesssteelwere
transgranular with multiple branching as shown in Fig. 14,
and this cracking mode was consistent with observations
reported in the literature for fatigue at 600C and below.
Differencesin the transgranular cracking associatedwith
stresscorrosion and fatigue have not been distinguished to the
extent necessaryto discern one mechanism from the other,
although the stresscorrosion cracks often are more numerous
and tend to follow crystallographic directions in the austenitic
stainlesssteels. In uniaxial fatigue tested specimens,cracks
were more+-less normal to the axial stresswith no
crystallographic preference. Composite floor tubes,of course,
are in a multiaxial stressstate, and cracking patternsunder
such stressesamdictated by the stressstate (19,20). Sincethe
superpositionof the thermal stresson the normal stressstate
of a pressurizedtube involves a degreeof nonproportional
loading, the direction of cracking in the tubes would be
difficult to correlatewith the cracking of uniaxially stressed
test specimens.
Transmission Electron Microscopy Microstructural
Studies
CXtenthe presenceof fatigue loads can be observedin the
dislocation substructureby transmission electron microscopy

1!5oox

1 soox

13.4

pm

l3.4pm

Figure 13 Metallurgical changes at the cladding interface of

a composite tube resultingfiom high temperature exposure:
(a) as-received; (b) afler 24 hours at 480 c.

Figure 14 Transgranular fatigue cracking ofJne-grained

304L stainless steeI tested at I % strain range and 600 c with
a hoId time of 0.I h per cycle for 730 cycles.

(TEM), and information on 304 and 304L stainless steelsis

widely available in the literature (2 l-24). At high
temperatures(above600 C) and large strain ranges(above
1% strain range), it hasbeen establishedthat dislocation cells
or subgmins form whosedimensions can be correlated with
the cyclic stressrange(2 1). At lower temperaturesand small
strain ranges,however,the dislocation substructures
developedin fatigue are quite sensitive to testing conditions.
Planar arrays of dislocations,tangles, cells, and labyrinth
stmctures have beenreported under thermal/mechanical
loading conditions (22-24).
Previous studiesexaminedthe substructure in a fine-grained
304L specimenisothermally fatigued at 300C and compared
this substructureto that observedin 304L cladding from three
compositetubes that cracked in service (10). Two of the
tubes were in serviceover ten years, and the third tube was
removedafter 18 months. The isothermally cycled test
specimenrevealeda substructurewith a iow concentrationof
network dislocations and somef&e loops and stacking faults.
The specimenappearedto be in the early stagesof forming
cellular networks (about l-2 pm in diameter) characteristicof
fatigue deformation at large strains (21). In contrast, the
substructurenear the surfaceof the 304L stainlesssteel
cladding from the long-term service tubesconsistedof very
densedislocation networks similar to cold-worked (>20%
strain) stainlesssteel(25). The substructurein the composite
tubes was not judged to be comparable to the substructurein
the fatigued specimen. Studies of the compositetube exposed
for 18 months revealedthat the near-surfaceand mid-clad
substructuresdiffered. The near-surfacehad a dense
dislocation structurewith clearly defined cells. The midclad
substructureconsistedof a low concentration of loosenetwork
tangles. The cellular structure near the surfacewasjudged to
be an indication of fatigue loading. This finding stimulated
.more detailed studieswhich involved (a) TEM examinations
of an unexposedcompositetube, (b) determination of
hardnessprofiles through the cladding of new and exposed
compositetubes, (c) TEM examination of a thermally
fatigued test specimen,and (d) examination of tubing that
cracked after long-term service.
The TEM analysisof the new compositetube showeda much
larger difference betweenthe near-surfaceand mid&d
dislocation structuresthan observedin the exposedtube. As
before, the substmctmein the cladding was examinedat two
locations; near-surfaceand mid-clad. The near surface
location was within 0.13 mm of the exposedsurface,while
the mid-clad location was 0.8 mm below the exposedsurface.
The near-surfacesubstructureof the new tube, shown in Fig.
ISa, consistedof a very densenetwork of dislocations
including bands laying along Cl 1I> crystallographic
directions within the grains Such substructureis
characteristic of heavycold work. By comparison,the mid-

clad substructure, shown in Fig. 15b,consistedof a lowdensity dislocation network characteristic of mill-annealed
material. To confirm the severedifference in throughthickness microstructure, hardnessmeasurementswere made
acrossthe stainless steel layer. Consistentwith the observed
dislocation microstructural differences,the cladding of the

new tube was much harder at the surface (>366 Vicken

hardness)than at the mid-clad location (about 170 Vicken
hardness). The hardnessgradient was very steepnear the
surface. Hardnessprofiles were then determinedthrough the
cladding of one previously examined tube (18 month
exposure),and it was found that the near-h
badness
was in the 280-325 Vickers range, while the mid-clad
hardnesswas in the NO-200 Vickers range. The less severe
hardnessgradient in the exposedtube was consistentwith the
smaller difference in dislocation substructureobservedearlier
(10). The diminishing of the hardnessgradient through the
cladding would be expectedif the cladding were exposedto
fittigue which tendsto harden annealed microsbuctures and
soften cold-worked microstructures. The results of fatigue
testson annealedand cold-worked specimensat 600C
exhibited such a trend.
Experimental studiesof 304L under thermal/mechanicat
fatigue indicated that hardening could be more rapid if plastic
straining occurs in a region of temperatureand strain rates
where dynamic strain aging occurs and that substructureis
similarly influenced (22,23). A thermal/mechanical fatigue
experiment was performedon a fine-grained 304L specimen
to examine this phenomenon. The specimenwas thermally
cycled under 111restraint (0.5% strain range) between300
and 600C with a 0.1 h hold time at 600C. As indicated in
Fig. 16, the cycle-to-cyclehardening was more rapid than in
isothermal testsperformed at higher strain ranges
(approximately 0.7%) at both 300 and 600C. The TEM
investigation of the thermal/mechanical fatigue specimen
testedfor 200 cyclesrevealeda very densetangle of
dislocation networksand loops. The featuresB-ereuniformly

!:~
1

10

100

1ooa

10000

Cycle*

J&y-e I5 TEA4micrographs showing the difference in the

substructure studies; (a) near-surface; (b) mid-clad.

Figure 16 Comparisonof cyclic hardening under

thermal/mechanical cycling with isothermal strain cycling.

distributed throughout the matrix and cellular arrays were

absent (Fig. 17a). Another important detail was the high
concentration of kinks and jogs along individual dislocation
segments. The substructurediffered from the fatigue
substructure shown in Fig. 17b that was producedby
isothermal cycling at 300 C.
Examination of crackedcladding from additional long-time
exposed tubes revealedlittle-or-no gradients in substructure
from the near-surf&e to the midclad section. Roth the near~&ace and midclad substructures were qualitatively similar
to the substructureobservedin the thermal/mechanical teat
specimen in the sensethat loops and kinked dislocation
segmentswere presentin both types of specimens. Overall,
the dislocation density was lower in the exposedcladding
than -in the thermally cycled specimen. Specimenswere
examined from the cracked and uncracked regions of the
z
cladding, and the substructures were found to be

Clearly, the microstructure and mechanical properties of the

304L cladding changedsigniticantly during service relative to
the as-manufacturedcladding. Further, there is some
evidencethat thetmal/m&.anical cycling is a major factor in
causing thesechanges. However, the rate at which
thermaVmechamcalcycling modifies the substructureis not
yet known. More importantly, the role that the substructure
plays in the developmentof cracking has yet to be established.
Stress Corrosion Cracking Studies
In parallel with the thermal fatigue studies are studiesto
identtfy environmentslikely to causeSCC of the outer 304L
stainlesssteellayer on composite tubes. Recentstudies have
concentratedon mechanismsthat can causecracking at
temperaturesbelow tube operating temperature;,i.e. during
water washes,shutdownsor startups. Most of the
experimentshave beenconducted with U-bend specimens
madefrom strips of 304L. The strips were approximately

Figure 17 TEM substructure produced by fatigue testing ofjne-grained 304L stainlesssteel (a) thermal/mechanical cycling
between 300 and 600 c with 0.5% strain range; (b) isothermal cycling at 300 c and 0.7% strain range.

3 mm (-l/8 in.) In thickness and about 93 mm (3-2/3 in.)

long. C-rings cut from a variety of compositetubeshave also
been used. The stressesin the specimenswere not measured,
but all were stressedpast the yield point. The procedure
followed was to cover the stressedportions of the specimens
with the salt, and then heat to the desired temperaturein a
mufIle furnace for a length of time that varied from 24-?O
hours.
These studies have shown that SCC will occur in 304L
stainless steel in pure molten hydrate of sodium sulfide,
Na.$9H,O or a mixture of Na$9H,O + NaOH, where the
NaOH content varied from O-10 wt%. The cracks which
formed in these teststypically followed a transgranular path
(Fig. 18). The principal direction in which the cracks
propagatedwas perpendicular to that of the applied stress,but
cracks often branched at a 45 angle hear the mid-point of
the specimenthickness.

Similar C-ring testshave beenconducted on a number of

other boiler floor materials, including Sanicro 38 (modified
Alloy 825) on carbon steel, carbon steel tubing with a weld
overlay of 309L or Alloy 625, and centrifugally cast, then coextruded, 3 10 stainless steelon a Cr-Mo alloy steel core.
Resistanceof thesealloys to SCC was asses& simply by
comparing the lengths of the cracks produced after 24 hours
exposure. The 304L and the 309L showed poor resistance,
and the cracksprogressedvery close to or all the way to the
interface (1.6-1.8 mm). In the 3 10 stainless, the longest
crack wasapproximately 325 pm. In the modified 825 alloy,
cracks were less than 50 pm in depth. No cracks were found
in Alloy 625 or one sampleof carbon steel that was testedThesetestswere conductedto examine the possibility that
SCC of compositetubes could be occurring during a dry-out
fire, or start- of a boiler after a water wash. It was
postulatedthat the surfaceof the tubes under those conditions
would be coveredwith a highly concentratedsolution
containing the salts present in remnants of the smelt bed.
The resultsare significant becausethey demonstratethat
rapid initiation of stresscorrosion cracks is possible when
they are exposedto an environment thought to be realistic,
within a temperaturerange where finite element analysis has
calculatedthat large tensile stresseswill be present on the
surfaceof the tubes. Additional experiments are planned to
better quantify SCC under theseconditions, and to explore a
range of salt chemistry which promotes SCC.
Analysis of Wash Water Samples

Figure 18 Micrograph showing cracks in 304L stainlesssteel

as a result of exposure in pure NaJ*SH,O at 16.5c for 16.5
hours.
In tests at temperaturessignificantly below the boiling point
of the salt (- 150C) SCC did not occur, nor was it observed
at temperaturesabovethe boiling point (-200C) where the
salt will quickly dry. SCC only occurred at temperatures
approaching ihe boiling point of the hydrated salt, that is
about 170C. It was also found that it could be promotedby
repeatedly heating the hydrated salt aboveits boiling point,
then cooling and rehydrating the salt by adding a small
volume of water.
In C-ring testsof 304USA210 compositetubing in a salt
mixture of 90% Na$9H,O + 10% NaOH, the progressionof
cracks in the 304L was quite rapid; cracks reachedthe
stainless steel/carbonsteel interface in a 48 hour test. In ail
the tests conductedthus far, there has not beena single case
where a crack has proceededacrossthe interface betweenthe
stainless steel outer layer and the carbon steel core.

Since the presenceof an aqueoussolution of Na,S would only

be expectedduring a time when water had been introduced
into the boiler, samplesof wash water were collected and
analyzedto determine the concentration of Na,S and other
compoundsof interest. The results of the analysis of one set
of samplesfrom a mill in the southeasternU.S. (26) are
shown in Table 1. These results indicate that the pH of the
wash solution remained fairly constant with measuredlevels
ranging from 11.5to 11.9, while the concentration of many
componentsdecreasedwith time. The sullide concentration
was quite low (Ul. loA) and remained fairly constant with
time. The table also showsthe approximate floor tube
temperatureat the time the sampleswere being collected.
Thesedataindicate that for this particular boiler, the floor
tube temperaturewas around 80C at the time wash water
reachedthe boiler floor. Consequently,during the initial
stagesof the shutdown conditions did not exist for SCC to
occur by the mechanismdescribedin the previous section.
Additional wash water sampleshave been or will be collected
and analyzed,and these results will significantly expand the
data baseon this material.

Table I Washwater sample analysis results as a function ofjloot tube temperature during the water wash.:
Temperature
(C)
2.36

57

80.6

3.1

1.70

5.59

16.9

1 0.054

2.64

1.32

5.78

17.3

0.020

11.6

2.75

0.66

5.96

17.8

0.019

11.6

4.25

12.2

1 0.054

11.7

11.7

1.88

0.35

1.53

0.21

4.89

14.2

1 0.031

11.6

1.89

0.17

4.33

12.2

1 0.032

11.7

1.57

1 0.13

5.18

14.6

1 0.039

11.7

1.42

1 0.10

3.44

9.2

1 0.054

11.9

Smelt Corrosion Studies of Alternative Materials

Information accumulatedto this point strongly suggeststhat a
materia.lother than 304L stainless steel will likely be required
for the surfaceof floor tubes exposedto the boiler
environment. One consideration in the evaluation of
alternate materials will be their resistanceto general
corrosion in the most extreme environment expectedto be
seenby a boiler floor, molten smelt. Tests were conductedin
a polarization cell constructed especially for molten salt
studies and usedsmelt with a nominal composition of 70 wt%
Na,CO,, 22 WV??
Na,S, 4 wt% Na,SO,, and 4 WI% KC1(27).
Corrosion rates measuredusing a polarization resistancetest
are shown graphically in Fig. 19. Alloy 825 and 304L
stainless steelfollowed by several iron-base high Cr alloys
had the lowest corrosion rates in testsin typic& smelt.

compositefloor tubes. A material can be selectedthat does

not experiencecracking in the environment of a boiler floor.
However, a completeand comprehensiveunderstandingof the
cracking mechanismhas not yet been reached. On the other
hand the problem can be addressedfrom anotherdirection
since tensile stresses,possibly as high as the yield strengthof
the stainlesssteel, are essential for cracking to occur. Either
a tube design could be adoptedin which distinct layersof
different composition are not present, or a material could be
selectedfor the outer layer such that tensile stressesdo not
developduring operation. In order to identi@ acceptable
materials for the outer layer of bimetallic tubes,a modeling
study has been initiated.

In a previous section of this paper, FE calculanonswere

carried out for co-extruded 304USA2 10 compositetubesin
three different thermal transient conditions. There are other
A second seriesof corrosion testswas also conductedin a
materials that will be consideredin the futuw, weld overlay
309L/SA2 10, coextruded Alloy 825&Q 10,weld overlay
lower melting tempemture smelt containing higher
Alloy 625karbon steel, co-extruded qlloy 625fSA210,
concentrations of potassium and sulfur in order to havea
composition more like that reported by Koivisto and Kiiskila
chromized carbon steel, and, possibly, other combinationsor
(9) to be present immediately adjacentto floor tubes. Results : metal sprays. Instead of performing numerouscalculations
ofthese testsare shown in Fig. 20. This smelt was
for different material combinations, a responsesurface(RS)
considerably more corrosive, and the iron-base high Cr alloys
study was initiated to provide a genera&d solution of the
had the lowest corrosion rates.
problem. The stressresponseat someparticnlar locationsin
the tube to variations in somematerial parameters[coefficient
of thermal expansion (CTE) and yield stress,aJ was
CONSIDERATIONS IN THE SELECTION OF
ALTERNATIVE MATERIAL!3
evaluated. A defined range of material parameterscoversthe
currently used materials as well as most engineering
Several approachescan be used to prevent cracking of
materials which might possibly be usedas alternativeoverIay

Figure 19 Corrosion rates of selected alloys in typical composition molten smelt.

4000
3500

p 3000
-% 2500
2
d 2000
f
i

IS00

e
4 1000
500
0

I+-t6Cr-2SI

Fe36Cr-tfl

Fe-120.3Sf

626

FMMt

Ni(3jAl

626

304L

SA2fO

Figure 20 Corrosion rates of selected alloys in potassium-sulfur-rich molten smelt.

materials. The study will provide an answeron the desirable
overlay material characteristics for the optimum mechanical
behavior during boiler operation.
The following assumptionswere made in order to initiate the
RS analysis:
-SA210 carbon steel material was consideredas a basetube
material in all calculations,
-thermal properties of SA2 10 carbon steelwere consideredfor
the base material and for the overlay material for all thermal
analyses(assemblywelding and in-service heating),
-the sameresidual stressesfrom extrusion were usedfor all
-3
-yield stresswas assumedto decreaselinearly to 10 MPa at
12OOC,and

-the rangefrom 0.9x10 to 2.1~10 T was consideredfor

CTE and the range from 100 to 700 MPa was consideredfor
OY-

FE computationswere performed at nine CTE - oy which are

distributed inside the selectedCTE - oYregion accordingto
the RS computational design, called Rotational Central
CompositeDesign (28).
Calculations have been completedfor the temperature
transient from room temperatureto operating temperature
and back to room temperature. Figures 21a and b show the
calculated hoop stressesat the fireside surfaceof the tube
crown at service conditions and at room temperature,
respectively,as a function of CTE and oYof the overlay
material.

In order to avoid stressconditions under which stress

corrosion cracking or thermal fatigue could occur, tensile
stresseson the tube surfaceshould be avoided and stresses
should not exceedthe elastic limit anytime during service.
An evaluation of the Rs results was madeaccording to the
selectedcriteria; stressesare compressiveand smaller than
yield stress. This evaluation was basedon the hoop and axial
stresscomponentscalculated at the fireside surfaceof the tube
crown and at the fireside surfaceof the membraneduring a
normal operating transient (from room temperatureto
operating conditions and back to room temperature). The
result is presentedin Fig. 22 which shows the region (dark
shaded)of a recommendedoverlay material that always
satisfiesthe smaller than yield stress criterion, and satisfies
the compressivestress- in all casesexcept for the axial

stressesat the membranefIreside surf&e. By considering the

properties of the various alloys that are viewed as candidates
for the outer layer, it is clear that Alloys 825 and 625 satisfy
thesecriteria. Future calculations will evaluate the capability
of theseand other alloys to satisfy the yield stress and
compressivestress criteria.
750
650
550
a
25

450

ii
a350
P

250

0.8

4.0
Thermal

1.2

1.4

expansion

1.6
coeffident

1.8

20

22

[lo" 'C']

Figure 22 Region of recommendedmaterials in termsof CT??

and a-for the overlay material.

SUMMARY
2
*?EC-n

h62a
A225

ss3oe

ss104

La

1:2

r:r

fhmmal expansion coeftkbd

[I 0 I.?]

2>

ucfnr

Figure 21 Hoop stressesat service conditions and afler

service asfunctions of CTE and auofthe overlay material.

Although the causeof cracking in 304USA210 composite

floor tubes has not been determined, considerableprogress
has beenmadein characterizing the cracking, as well as in
defining the stressesdevelopedin tubes as a result of
operation. Information provided by mills and boiler
manufacturersconfirm that shortduration temperature
increasesdo occur on boiler floor tubes, and, whiIe these
fluctuations may usually have a magnitude of considerably
less than 5OC, fluctuations of 150 C or greaterdo occur
occasionally. In addition to the generally acknowledged
wide, tmnsgranular, relatively unbranched cracksthat are
seenin compositetubes, short, narrow, transgranular cracks
with somebranching are also present at the surfaceof the
stainlesssteel layer.
Finite element modeling predicts, and X-ray and neutron
difhaction studieshave confirmed, that tensile stresses
develop on the surfaceof 304USA2 10 tubesbelow the
operating temperatureas a result of thermal cyclesbetween
room temperatureand operating temperature. In areaswhere
thermal excursionsof sign&ant magnitude occur, tensile
stressescan developat operating conditions.

Basedon fatigue studies and TEM examination of samples,

the evidenceobtained to date doesnot support thermal fatigue
as the sole mechanism causing cracking of compositetube.
Examinations do indicate that previously exposedtubeshave
been subjectedto somethermal cycling such that someeffect
on properties has resulted.
SCC studies have shown that Na$9H,O causescracking in
304L stainless steel in laboratory testsin the 150-200C
temperature range. Tests are continuing on co-extrudedtubes
of different compositions, tubes with weld overlaysof
different compositions, and tubes with a diffusion applied
surf&e layer. Further testing will also be done to determine
if the stressesand compositions are representativeof those
experienced in recovery boiler floor tubes.
-Modeling studies have been initiated to define the rangeof
alloy properties (thermal expansion coeflicient and yield
strength) under which the stressesdevelopedon the surfaceof
a compositetube do not becometensile and do not exceedthe
elastic limit. Initial results for normal operating conditions
indicate that Alloys 825 and 625 satisfy these requirements.
These results suggestthat minimizing the magnitudeof hot
spots may keep the surface stressesin compositetubes
compressiveduring operation. It also appearsprudent to
avoid situations where wash water is allowed to remain in
contact with floor tubes, especially when the floor tubesare in
the temperaturerange of 150-200C.

Boilers: A State-of-the-Art Review, (1997).

2. Oral presentationby M.P. LeBel, ABB CE Servicesat
August 22, 1996review meeting for Development of
Materials for Black Liquor RecoveryBoilers, Laurel,
Maryland.
3. Private communication, J. May, Weyerhaeuser-CoIumbu,
Mississippi to J.R Keiser, Oak Ridge National Laboratory.
4. Private communication, K. Meissner, Georgia-Pacific,
Ashdown, Arkansas,to D.L. Singbeil, Pulp and Paper
ResearchInstitute of Canadaand 3. R Keiser, Oak Ridge
National Laboratory.
5. Presentationby MD. Moskal, StoneContainer Corp. at
June 13-15,1995, AFBtPA SeminarRecovery Boiler Lower
Furnace - What You Need to Know, Atlanta, Georgia.
6. Private communication, B.O. 0 scarsson,Fluor Daniel
Forest Products,Greenville, South Carolina, to J.R Keiser,
Oak Ridge National Laboratory.
7. Private communication, L. Koivisto, Ahlstrom Machinery
Corporation, Varkaus, Finland, to J.R Keiser, Oak Ridge
National Laboratory.
8. Private communication, MG. Fremont, PH. Glatfelter,
Spring Grove, Pennsylvania, to J.R Keiser, Oak Ridge
National Laboratory.

ACKNOWLEDGMENTS
The authors wish to acknowledgethe efforts of H.F.
Longmire for preparation of metallographic specimens,J.W.
Jonesfor selection and preparation of electron microscopy
specimens,P. Eng for conducting SCC experiments,D.F.
Wilson, S.J. Pawel, and J.R DiStefano for review of the
document, and ABB-CE Services,Inc., Sandvik Steel,and
Welding Services Inc. for contribution of much of the sample
material used for laboratory studies. Information, tube
samples,and assistancehave also beenprovided by ABB-CE
Sewices, inc., Ahlstrom Machinery Corporation, Babcock&
Wilcox, Kvaemer Pulping Technologies, Fluor Daniel Forest
Products, Champion International, Georgia-Pacific,P.H.
Glatfelter, International Paper, Irving Pulp and Paper,James
River, MacMillan Bloedel, Mead, Potlatch, Rivetwood
International, Union Camp, Westvaco,Weyerhaeuser,and
Weyerhaeuser-Canada.

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