S

SPE 1610
028

E
Effectiven
ness of Self-Heali
S ng Ceme
ent Additiives Base
ed on Tes
st
M
Methodollogy Usinng Simulaated Cem
ment Sheaath Crackks
R
Robert Brown
ning, Marcus Duffy,
D Drew Gaugler,
G Paul Jones, Hallib
burton

C
Copyright 2012, Society
y of Petroleum Enginee
ers

T
This paper was prepare
ed for presentation at the SPE Eastern Regio
onal Meeting held in Le
exington, Kentucky, US
SA, 3–5 October 2012..

T
This paper was selected for presentation by an a SPE program comm mittee following review of information containned in an abstract submmitted by the author(s)). Contents of the papeer have not been
re
eviewed by the Society y of Petroleum Engine eers and are subject to o correction by the autthor(s). The material ddoes not necessarily reeflect any position of the Society of Petroleu
um Engineers, its
officers, or members. Electronic
E reproductionn, distribution, or stora
age of any part of thiss paper without the wrritten consent of the S Society of Petroleum E Engineers is prohibite
ed. Permission to
re
eproduce in print is res
stricted to an abstract of
o not more than 300 words;
w illustrations mayy not be copied. The abbstract must contain co
onspicuous acknowled dgment of SPE copyrig ght.

AAbstract
A testing metho odology was developed to ex xamine the effeectiveness of oiil-swellable addditives in cement slurries by evaluating
thhe capability to
t shut off hyd drocarbon fluid d flow throughh a crack initiaated in the cemment. An openn-loop testing ffixture was
uused to investig o oil-swellablle additive conccentration and environmentaal temperature, using Kaydol mineral oil
gate the effect of
aas a test fluid. Under a pressu ure differential of approximaately 2 psi/in., test results inddicated that a concentration of 10% by
vvolume of addiitive relative to
o a 15.5 lbm/gaal Class G slurrry was sufficiennt to significanntly reduce hyddrocarbon floww in a crack
inn cement at a temperature of 160°F in an a average tim me span of 488 hr and in shhorter time sppans with an iincrease in
temperature.

Introduction
DDuring their seervice lifetime,, downhole cem ment sheaths area subjected too mechanical sstresses that caan result in faiilure of the
sstructural integ grity. For exaample, thermall and mechan nical cycling ccan deform thhe cement sheeath to the pooint where
mmicrocracks forrm throughoutt the annulus. TheseT microcraacks can serve as divergent fl flow paths for pproduction fluiid from the
wwellbore, resultting in not only y lost revenue,, but also rapid
d deterioration of the cement sheath as a ressult of propagaation of the
ccracks already present.
p
A typical solution to rem medy microcraccks that result in loss of zonnal isolation iss to perform a squeeze job. Cement is
““squeezed” through perforations in the casiing and cemen nt sheath in ann attempt to re--establish zonaal isolation. Beecause it is
ddifficult to deteermine exactly where the losss has occurred,, squeeze jobs do not alwayss remedy the siituation. An altternative to
pperforming rem medial squeeze jobs is to mod dify the mechaanical properti es of the cemeent so that the downhole sheeath will be
mmore durable anda resilient to better withstan nd the stressess that occur froom thermal/meechanical cycliing. One effecttive way to
mmodify the mecchanical properrties of cementt is to incorporrate elastomer pparticles.
When addeed to cement slurries, elastom mers lower thee Young’s moddulus, makingg the cement m more elastic (DDarbe et al.
22008; Wray et al. 2009). Thiis allows the cement sheath to t better mitiggate the stress aand strain statee encountered downhole.
WWhile the incorrporation of elaastomer particlles can lower the t compressivve strength of thhe cement, thee particles serve to absorb
aapplied stress anda can tough hen the cement sheath to preevent cracks ffrom propagatiing as extensivvely as if therre were no
eelastomers pressent (Segre et al. 2006). Theere is also a practical
p limit rregarding howw much elastom mer can be loaaded into a
pparticular slurrry design. As the elastomerr loading incrreases, the sluurry viscosity increases, whhich increases equivalent
ccirculating density (ECD) and d will ultimateely require slowwer pumping rrates to reduce the risk of unnnecessarily fraacturing the
fformation (Wraay et al. 2009).
In additionn to improving g the mechaniical property envelope, elasstomeric addittives provide an additional benefit of
inncreasing in siize by swelling when contaccted by hydroccarbon fluids. F Flory and Hugggins are well--known for deeveloping a
thheory on the in nteractions of elastomers witth organic solv vents that give way to swellinng (Billmeyer 1984). The theeory shows
thhat the chains of the elastom mers relax in thet presence of o the solvent m molecules. Ass a result, the elastomer voluumetrically
eexpands, or sw wells. Productio on fluids are laargely composeed of hydrocarrbon chains, annd, when thesee fluids flow tthrough the
ddivergent flow paths in the ceement sheath created
c by craccks, they can aact as solvents and activate thhe volumetric sswelling of
thhe particles at the interfacess of the crack. When the particles have sw welled to a sizee close to the ccrack size, the crack will
eeventually be filled
fi and a seall will be formeed, thus shutting off flow of thhe divergent prroduction fluidd.
The capabillity of the elasttomeric particlles to shut off flow
f is dependdent on particlee size, crack sizze, and chemiccal makeup
aand temperaturre of the well fluid.
f If the elastomer particle size is too ssmall relative to the crack w width, the swellling of the
2 SPE 161028

elastomer will not be sufficient to fill the volume created by the crack. With regard to well fluid chemistry, if the organic
solvent contains aromatic groups or compounds, the swelling activity of the elastomer is typically more vigorous
(Chandsekaran 2010). Because the backbone chains of elastomers contain double bonds, the double bonds present in the
aromatic groups allow for more interaction between the solvent molecules and the elastomer particles. Furthermore,
temperature plays an important role in driving the kinetics of the swelling action of the elastomer. The well-known Arrhenius
law (Eq. 1) shows that kinetic processes experience an exponential increase in rate with respect to a linear increase in
temperature.

k = A•e-E/RT .................................................................................................................................................. (1)

where k is the rate constant, A is a coefficient, E is the activation energy, R is the universal gas constant, and T is the
absolute temperature.
A previous test method was created where a cured cement cylinder containing a swellable elastomer additive was cut in
half and reassembled inside a smooth-walled testing sleeve to simulate a crack (Darbe et al. 2009). The testing cell was
modified from a standard static fluid-loss setup. Mineral oil was used as a test fluid to flow through the simulated crack, and
the flow rate was monitored to observe when flow shutoff had been achieved. While the results of the previous work are
plausible, it was desired to show the same capability of shutting off hydrocarbon fluid flow using a microcrack similar to
what would be expected in a downhole cement sheath.
This paper illustrates a modification of the previous test setup where the sample was physically cracked in such a way as
to better represent an actual downhole crack. The procedure for preparing samples is described and the effects of elastomer
loading, fluid temperature, and the strength of the seal formed by the elastomer are discussed.

Experimental Details
Sample Details. The slurry design for this study consisted of a 1.87 SG (15.5 lbm/gal) slurry. The slurry designs are given in
Table 1 and incorporated the same swellable elastomer as used in Darbe et al. (2009), with a content ranging from 0 to 20%
BWOC, as well as other additives. A weighting agent was incorporated to maintain the SG as the elastomer content
increased. Before mixing the slurries, red lithium grease was applied to the inside wall of a testing sleeve. A plastic cap was
placed on the end of the sleeve without the lip, and black electrical tape was wrapped around the edge of the cap to seal
against water leaking into the cell during curing. The mixed slurry was then poured into the sleeve. A greased metal cap was
placed on top of the testing sleeve to seal the top. Samples were cured overnight in a water bath at 122°F.

TABLE 1—SLURRY FORMULATIONS (DENSITY = 15.5 lbm/gal)

Loading, % BWOC
Slurry component
Slurry A Slurry B Slurry C Slurry D Slurry E
Water 43.1 43.1 43.1 43.1 43.1
Class G cement 100 100 100 100 100
Weighting additive 2 6 13 21 29
Swellable elastomer 0 5 10 15 20
Fluid-loss additive 0.5 0.5 0.5 0.5 0.5 

Testing Setup. All tests for this work were performed using an open-loop test setup (Figs. 1 and 2) consisting of a fluid
reservoir pressurized with nitrogen and three stations, each equipped with two standard static fluid-loss cells (FLC), and each
with heating jackets equipped with temperature controllers, thermocouples, and a bucket placed on a scale for fluid
collection. The scales were connected to a computer for data collection to track the flow rate.
S
SPE 161028 3

Fig. 1—Open-loop test se

etup.

Fig
g. 2—Flow diagram of the open
n-loop setup.

For each staation, the two FLCs

F ne FLC was ussed to preheat tthe test fluid before entering the second
were useed in series. On
FFLC, which heeld the samplee. The FLC ho olding the sam mple was preheeated to the same temperatuure as the oil to prevent
thhermal shock. The componeents of the FL LC for the testt sample can bbe seen in Figg. 3. The test sample (Fig. 3c) with a
ddiameter of 1.7 75 in. and thicckness of 1 inn. was placed inside
i the testting sleeve (Fiig. 3d), which was lubricateed with red
liithium compleex grease. A brrown Viton O-ring (Fig. 3f) covered
c in siliccone vacuum ggrease and wass placed on eitther side of
thhe sample, folllowed by a sprring/washer combination (Fig g. 3b). The edgges of the washhers were beveeled to establish a contact
aarea between the t washer and d O-ring. The purpose of th he spring/washher combinatioon was to seat the O-rings thhrough the
ccompressive acction of the sprrings when the lid of the FLC C was threadedd down. This hhelped ensure tthat flow was tthrough the
ccrack in the sam mple by preven nting flow arouund the edges. The black Vitton O-rings (Fiig. 3e) were plaaced on either side of the
liip of the testing sleeve (Fig. 3d)
3 to seal the lid of the FLC C.
4 S
SPE 161028

Fig. 3—Com
mponents of flu
uid-loss cell hollding the test sa
ample.

SSample Preparation Proced dure. To simullate a realistic crack in a cem ment specimen,, a “score and bbreak” methoddology was
ddeveloped:
1. Remov ve the testing sleeve assembly used to curee the sample fr from the water bath. Removee the metal capp, electrical
a plastic cap from the sleev
tape, and ve (Fig. 4b).
t cured cemeent sample out of the testing sleeve
2. Push the s (Fig. 4c)).
3. From the cylindricall sample, cut samples
s that arre 1-in. thick ((Fig. 5a) and pplace them in a container w with enough
water to cover the reesulting cut sam mples.
4. Using a fine-blade saw (coping saw w or hacksaw), cut a 1/8-in. deep notch in the middle of one side of thee specimen
(Fig. 5b).
5
5. Place the sample, wiith the crack faacing downwarrd, on a surfacce with two staationary points positioned on either side
of the crack, as showwn in the schem matic of Fig. 5cc.
6. Positio on a metal rodd (1/2-in. diameeter) directly over
o the notch on the side of the sample faccing upward (F Fig. 5d). In
this ex
xample, a FLC preparation staand was used to t provide the ttwo stationary points on eitheer side of the ccrack.
7. Hold thet rod againstt the sample facce with one haand, and, with tthe other hand,, hit the rod firrmly with a ham mmer (Fig.
5d).
8. After the crack has propagated
p and h been brokeen, the halves oof the sample can be pulled apart (Fig.
d the sample has
5e).
9. Any fragments
f or particulates rem maining from cutting
c the nottch should be washed off, aas these might artificially
contribbute to flow shhutoff and skew w experimentall data.
10. Observ ve that the cracck is fairly unifform and has propagated
p throough the approoximate center of the sample (Fig. 5e).
11. After applying a fresh coat of red grease to the testing sleeve,, reassemble thhe halves and place them baack into the
g sleeve. O-rin
testing ngs and seatin ng springs aree then placedd on either sidde of the sam mple to prevennt flow of
hydroccarbon fluid arround the annular space of thee sample insidee the testing sleeve.
12. The teesting sleeve iss then inserted into the FLC, and the testinng setup is asseembled. The hhydrocarbon fluuid and the
samplee inside the reespective FLC Cs are then preeheated to thee same temperrature by applyying heat to tthe heating
jackets.
13. After preheating,
p flu
uid flow is starrted. After it fllows through ththe sample, fluuid is collectedd on a bucket pplaced on a
scale, which is conn nected to a com mputer. A softwware program iis used to monnitor the mass fflow rate as a ffunction of
time. The
T SG of the fluid is used to o convert mass flow rate to voolumetric flow w rate.
S
SPE 161028 5

(a
a) (b) (c)

F
Fig. 4—Compon nents of curingg cell used in experiment:
e a) assembled
a curiing cell, b) dis assembled celll with sample rready to be
p
pushed out of te
esting sleeve, an
nd c) cured sam
mple pushed out of testing slee
eve.

Fig. 5—
—Steps involve
ed in the “score and break” pro
ocedure for sam
mple preparation
n.
6 S
SPE 161028

RResults and Discussion

D
TThe maximum flow rate during the experim ment was recorrded as the inittial flow rate aand was used tto normalize alll flow rate
ddata points. Th
he absolute and normalized flow rate dataa points were pplotted againstt time to obseerve the capabiility of the
eelastomer to sh
hut off fluid flow through sweelling action.

EEffect of Elasstomer Loadin ng on Shutofff Capability. Because of tthe nature of the crack proopagation throuughout the
ssamples, this tyype of testing is
i inherently un nrepeatable in terms of absollute flow ratess through a sammple. To comppare sample
vvariability, all flow rates werre normalized to determine th he relativistic nature of the eelastomer loadding. To investtigate what
looading was required to signiificantly reducce flow shutofff, tests were coonducted with samples contaaining 0, 5, 100, and 20%
BBWOC swellab ble elastomer additive. Figs. 6 and 7 illu ustrate the absoolute and norm malized flow rrate of samplees tested at
1160°F with a pressure differeential of about 2 psi/in. Previously, it was sstated that the ssamples were ccured at a tempperature of
1122°F. Normally, samples aree cured at the temperature at which they willl be tested. In this case, the samples were aall cured at
thhe same tempeerature to maxiimize testing th hroughput. However, some ssamples were ccured at the tessting temperatuure and, for
thhe purposes off this work, teesting a samplee at a higher teemperature thaan the curing ttemperature diid not appear tto impart a
ssignificant diffeerence in the reesults.
If more elasstomer particlees are incorporrated into the slurry,
s a crack should be ablee to be sealed more effectiveely through
thhe volumetric swelling actio on of the particcles. It can be gathered
g from the results in Fig. 7 that a cement slurry wwith a final
ddensity of 15.5 5 lbm/gal incorrporating a min nimum of 10% % BWOC of ellastomer additiive should be able to reducee fluid flow
thhrough the sam o the equipmeent used in this experiment inn an average tim
mple to a level below the deteectable limits of meframe of
aabout 2 days att 160°F. It wass noted that sm maller and larg ger elastomer looadings were aalso able to acchieve similar rresults, but
thhe timeframe ini which this occurred was diifferent.

F
Fig. 6—Absolute
e flow rate as a function of time
e for samples containing vario
ous loadings of s
swellable elasto
omer tested at 1
160°F.
S
SPE 161028 7

F
Fig. 7—Normaliz
zed flow rate as
s a function of tiime for samples
s containing varrious loadings o
of swellable ela
astomer tested a
at 160°F.

EEffect of Tem mperature on Shutoff Beha avior. Tests were

w conductedd on samples containing 100% BWOC ellastomer at
temperatures off 80, 120, 160,, and 190°F. The T tests condu ucted at 80°F w were performedd for approxim mately six dayss, while the
oother tests weree performed for one day. Figss. 8 and 9 show w the test resullts for all sampples for comparrative purposess, and Fig.
110 shows the 80°F
8 normalizeed flow rate reesults for the full
fu time scale. The data show w that a higheer temperature resulted in
ffaster flow shuttoff. The curvees appear to shoow an exponen ntial decrease oof flow rate with respect to time. As such, eexponential
he time requireed to achieve fflow rate reducction to essenttially 100%. Thhe average
trrend lines werre fit to the datta to extract th
tiime required to achieve this behavior at eaach temperaturre, as well as tthe initial flow w rates of all saamples, is sum
mmarized in
TTable 2. Fig. 11
1 shows a sem milog plot of timme as a functio on of inverse ttemperature. Thhe fit of an expponential trenddline to the
ddata shows thaat the observed d temperature effect on the shutoff capabiility of the elaastomer additivve follows the Arrhenius
rrelationship meentioned previiously. From theset results, the activation energy of the elastomer caan be calculatted as ~27
kkcal/mol.
8 S
SPE 161028

F
Fig. 8—Absolutte flow rate as
s a function off time for sam
mples containin g 10% BWOC swellable elas
stomer tested at different
te
emperatures.

F
Fig. 9—Normalized flow rate as
a a function of
o time for sam
mples containin
ng 10% BWOC
C swellable elas
stomer tested at different
te
emperatures.
S
SPE 161028 9

TABLE 2—INITIAL FLOW RATES

R AND AVE
ERAGE PREDICCTED TIMES TO
O SHUT OFF 100
0%
OF HYDRROCARBON FL LUID FLOW AT EACH
E TEST TEMMPERATURE F OR SAMPLES
CONTAIN
NING 10% BWOOC SWELLABLE E ELASTOMER
Average Shutoff
Temperatu
ure Initial Flo
ow Rate, mL/min Time, h
hr
Sample A 1.8
80°F Sample B 1.2 36,472
2
Sample C 1.7
Sample A 0.6
120°F Sample B 1.2 555
Sample C 0.2
Sample A 16.9
160°F Sample B 0.4 42
Sample C 9.7
Sample A 3.8
190°F Sample B 0.5 7.6
Sample C 7.9

F
Fig. 10—Full tim
me-scale plot of normalized flow
w rate of sample
es containing 10
0% BWOC swelllable elastomerr tested at 80°F.
10 S
SPE 161028

Fig. 11—Logarithm
m of time to shut off hydrocarbo
on fluid flow as
s a function of in
nverse absolute
e temperature.

EEffect of Presssure Increase on Swollen Elastomer

E Seall. Once the elaastomer particles have swolleen sufficiently to shut off
ffluid flow, it is possible that a sudden increase in downho ole pressure couuld affect the sstrength of thee seal that has fformed. To
eevaluate this, a separate samp ple containingg 10% BWOC of elastomer w was tested at 1160°F. After shutoff was observed, the
ppressure differeential was incrreased from ~2 2 psi/in. to 12 psi/in.,
p wed to continuue. The results in Fig. 12
and thee test was allow
sshow that, if a crack was seelf-healed by the t swollen elaastomer partic les, a pressuree differential iincrease of 10 psi/in. re-
eestablished flow w. When the pressure
p was deecreased back to the originall magnitude, noo self-healing was observed,, indicating
thhat a shutoff of flow was nott attainable.
Even thoug gh fluid flow was
w re-establish hed and no sub bsequent self-hhealing occurreed, the magnittude of the flow w rate was
ssignificantly loower than the initial flow raate. The resultts in Fig. 12 show that an increase of 10 psi/in. of thhe pressure
ddifferential onlly increased thhe flow rate too 10% of the initial flow ratte, and reducinng the pressuree differential bback to the
innitial magnitud de lowered it to approximattely 2.5% of th he initial flow
w rate. Based oon these results, it was conccluded that,
wwhile self-healiing after flow has been re-esstablished might not be posssible, the reducction in flow relative to the iinitial flow
rrate would still be beneficial to
t the overall liife of the well.
As stated previously,
p the purpose of thiis paper is to introduce
i a moodification of an existing methodology thaat allows a
ccement samplee to be tested with a crack that mimics a downhole craack. This moddification, whiile a realistic ssimulation,
yyielded inheren ntly unrepeatab ble results and
d should only be b used to show w the functionnality of the ellastomer to shuut off fluid
fflow through sw welling in a microsized
m crack
k. To gain morre fundamentall, scientific inssight into the m material behaviior, a more
rrepeatable test method is necessary. Furth hermore, the reesults shown iin this work aare, at best, coonservative esttimates. As
sstated, the arom matic content of the hydroccarbon fluid willw play a signnificant role inn the swellingg action of thee elastomer
pparticles and thhus the flow shuutoff capability
y. This is the fo
ocus of a futuree study.
S
SPE 161028 11

F
Fig. 12—Plot of normalized flow
w rate as a functtion of time with
h pressure incre
eases to test th
he strength of th
he swollen elasttomer seal.

CConclusions
A method for establishing
e fluuid flow throuugh a cement sample
s was deeveloped that mmimics the forrmation of a ccrack when
ccement is placeed under stresss. Variations in
n swellable elaastomer loadingg and fluid temmperature weree conducted too determine
thhe effects of these
t variabless on the cemen nt sheath’s ab
bility to heal. A According to tthe results from tests perforrmed using
KKaydol white mineral
m oil as a test fluid, a loading of 100% BWOC sw ellable elastom mer additive inn a 15.5-lbm/ggal Class G
ccement is suffficient to shut off fluid flow w at 160°F in n an average timespan of aapproximately two days at a pressure
ddifferential of approximately 2 psi/in. Furthermore,
F he time requiired to shut off fluid flow
th w appeared too decrease
eexponentially with
w a linear in ncrease in temp perature. If an increase in prressure differenntial occurs aft
fter fluid flow sshutoff has
bbeen achieved, the seal formmed might be co ompromised and
a flow couldd be re-establisshed. In this caase, the magniitude of re-
eestablished flow
w would be sub bstantially low
wer than the inittial flow rate.

AAcknowledge ements
T on for permissiion to publish this work andd Dr. Benjaminn Iverson for iinput on testinng and data
The authors thaank Halliburto
rreporting.

R
References
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Billmeyer, F.W. 1984. Textbook of Polymer Scieence. New York, New York: Johhn Wiley & Sonss. doi: 10.1002/ppol.1984.130221210.
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Chandsekaran, V.C.
V 2010. Rubbeer Seals for Fluiid and Hydraulicc Systems. Oxforrd, United Kingddom: Elsevier, Innc.
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Darbe, R., Gordoon, C., and Morggan, R. 2008. Slu
urry Design Con nsiderations for M
Mechanically Ennhanced Cementt Systems. Paperr AADE-08-
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Darbe, R., Pewittt, K., and Karch
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Segre, N., Ostertag, C., and Mo onteiro, P.J.M., 2006. Effect off Tire Rubber P Particles on Cracck Propagation in Cement Pastte. Materials
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Wray, B., Bedforrd, D., Leotaud, L., and Hunter, B. 2009. The Application
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High-Density Elaastic Cements to Solve HPHT Challenges in
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S Paper SPE
E 122762 presen nted at the SPE AAnnual Technicaal Conference annd Exhibition, N
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U 4–7 Octob
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