J181347 DOI: 10.
2118/181347-PA Date: 31-May-17 Stage: Page: 1
Rheological Characterization of
Suspension of Hollow Glass Beads
Simone Lumsden, John P. Singh, Ronnie G. Morgan, and Gregory Hundt, Halliburton
Summary
Hollow glass spheres (beads) are widely used as density and rheo-
logical modifiers for various oil and gas process fluids, particu-
larly cement. One of the primary uses is to achieve lightweight
slurries with good mechanical properties of the set cement. This
paper discusses a concentrated, yet pumpable, suspension of these
spheres for offshore cementing applications. Providing the light-
weight spheres in a liquid suspension eliminates the risks associ-
ated with dry blending these materials. The development of the
liquid suspension of hollow beads enables on-the-fly mixing of
cement slurries with desired density profiles.
Currently, the beads are premixed in the cement powder before
they are shipped to offshore locations, which could result in the
segregation of the beads during delivery and storage, and limits
operations to the predetermined density (concentration of beads)
of the slurry. This paper presents the rheological behavior of the
concentrated suspension (up to 60% vol/vol) of hollow glass
spheres suspended in a dilute aqueous solution of bentonite and
soda ash. In addition, an attachment to the viscometer (called
Fann Yield Stress Adaptor or FYSA) was used to characterize the
flow behavior. A rheological model was developed to highlight
the bead/bead surface interactions as a major component control-
ling flow behavior.
Four different variants of beads were studied. These were
selected to represent a range in surface area per unit volume of
beads. Increasing the concentration of beads or the bentonite in
solution correlated to increased yield stress and fluid viscosity at
operational shear rates. In addition, a Krieger-Dougherty-type
relation captured well the effect of the bead concentration, with
the maximum packing fraction of beads as a function of surface
area per unit volume of the beads. Overall, the Herschel-Bulkley
(HB) model best described the suspension rheology with the
shear-thinning exponent in the range of 0.8 to 1.0. Surface area
of the beads linearly correlated to the yield stress of the corre-
sponding concentrated bead solution.
Results of this study and the model developed can be used to
develop variants of the system with minimal experimentation,
thus significantly shortening the design time.
Introduction
Cement slurries for oilwell applications are required to exert the
optimal level of pressure on the formation. The stress (or pres-
sure) should be greater than the pressure exerted by the formation
fluids and lower than the net strength of the walls of the forma-
tion. The primary force that the cement slurry (or any other dril-
ling/completion fluid) will exert is caused by the hydrostatics.
Thus, density is the primary surrogate property by which a ce-
menter is able to tune the forces experienced by the formation
walls. Depending on the formation, the density can range from
20 to 22 lbm/gal at the higher end to 8 to 10 lbm/gal at the
lower end.
To achieve lower densities (less than approximately 11 lbm/
gal), one should either foam (Benge et al. 1982) the slurry or add
hollow beads/glass microspheres (Tanner and Harms 1983) with
Copyright V
C 2017 Society of Petroleum Engineers
This paper (SPE 181347) was accepted for presentation at the SPE Annual Technical
Conference and Exhibition, Dubai, 26–28 September 2016, and revised for publication.
Original manuscript received for review 1 September 2016. Revised manuscript received for
review 1 February 2017. Paper peer approved 3 February 2017.
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density comparable to or lower than water to the formulation.
There are some other additives, such as zeolites (Fyten et al.
2005), clays, and forms of silica (Kulkarni and Hina 1999) with
high surface area that can be used to adsorb water to stabilize the
slurry formulation at low densities. However, their use is gener-
ally limited to slurries with formulation densities greater than
11 lbm/gal.
When designing slurries with hollow beads, several things
should be considered. Primary among those is the fact that, at
such low densities, the solids-to-water ratio (SWR) is a sensitive
function of the slurry density (Kulakofsky and Vargo 2005; Tan
et al. 2012). Cement is formulated to provide appropriate zonal
isolation under downhole conditions. SWR is one of the primary
variables that govern the mechanical properties of the set cement.
Thus, any significant variations in SWR should be minimized.
Tan et al. (2012) have shown that “volumetric based” mixing is a
preferred method for preparing lightweight beaded slurries at such
low densities compared with the density-based control that is gen-
erally applied at the mixing tub. In addition, inline solid-powder
delivery is relatively more challenging to control compared with
the inline liquid delivery.
State of the art is to preblend the hollow beads in the cement at
the desired concentration and then deliver the blend to the rig. This
process limits the operations to one predetermined density. In
addition, there might be a significant segregation of beads caused
by multiple pneumatic transfers. As the blend is removed from the
bottom, the initial cement blend may be deficient in beads,
whereas the final cement blend withdrawn might be too rich in
beads. As noted, the rig-operations control systems monitor the
density, and hence, the control system will compensate the lack of
beads in the blend by adding water to the initial mix, possibly mak-
ing it unstable, whereas the amount of water in the later stages
might be too low for efficient mixing. The presence of too much
water can affect the mechanical properties of the set cement,
whereas the water-starved slurry will contribute to higher equiva-
lent circulating densities (ECDs) through increased hydraulic fric-
tion. Both of these extremes add risk to the operations.
These outlined reasons combined with the fact that offshore
rigs prefer handling liquid additives inspired efforts to develop a
stable “liquefied” version of the hollow beads (Kulakofsky and
Vargo 2005; Abdullah et al. 2013; Maxson et al. 2016). A pump-
able concentrated solution of beads when mixed with cement
slurry on the fly at the rigsite circumvents many of the aforemen-
tioned challenges of handling the powdered blend containing hol-
low beads. When executed appropriately, liquefied beads should
provide significantly more effective control of the SWR in the
cement slurry and, hence, better control over mechanical proper-
ties of the set cement, resulting in the designed performance. It
also helps prevent the issue of segregation of beads, provides
improved control over the density of the slurry being pumped,
and results in operational flexibility.
To achieve these desired results, the key is to have a liquefied
bead suspension that minimizes bead segregation while maintain-
ing the flowability so that the system can be pumped. After a sta-
ble formulation is achieved, the pumping requirement is from the
storage tank to the liquid-additive system pump to then be intro-
duced into the cement slurry. These pumping requirements could
vary significantly between rigs and will need to be considered for
successful operations.
In this work, a simple, yet effective, formulation of the
“liquefied beads” was developed, and then rheology was
1
 J181347 DOI: 10.2118/181347-PA Date: 31-May-17 Stage: Page: 2 Total Pages: 10

Table 1—Particle size of the various beads used. Surface area (SA) has been normalized with that of B2 beads. Span is defined as d50/
(d90 2 d10). LMD is the log mean diameter.

characterized as a function of various constituents. In the simplest
formulation, beads are added to an aqueous medium, and a sus-
pending aid was used to minimize any segregation. The role
played by the concentration of the suspending aid and concentra-
tion of the beads on the rheology was characterized. Four different
kinds of beads were used in the formulation to quantify effects of
particle size and distribution on flow behavior. A model to capture
the effects of these various parameters on suspension rheology
was developed.
It was found that the shear-dependent rheology of the suspen-
sion can be appropriately described by the HB model with the
power-law index (n) between 0.8 and 1.0. At a fixed shear rate,
the Krieger-Dougherty form was found to describe the depend-
ence of viscosity on the beads volume fraction in the suspension.
Generally, the Krieger-Dougherty form is used to describe the
particle-concentration dependence of viscosity of suspensions in a
Newtonian medium (e.g., Mueller et al. 2010). In contrast, the
suspending phase in this work is a shear-thinning solution of ben-
tonite in aqueous medium. In addition, it was found that the
viscosity at a fixed shear rate could be described by a phenomeno-
logical model with three terms: a linear dependence on bentonite
concentration, Krieger-Dougherty form to capture the bead con-
centration, and a term that depends on the surface area per unit
volume of the beads.
Experimental
Materials. The hollow glass beads used in this work were all
obtained from the 3M Company. The beads are marketed under
the trade name of 3MTM Glass Bubbles. The beads were charac-
terized for particle-size distribution (PSD). Four different prod-
ucts were considered in this study. They were chosen to provide a
range of surface area per unit volume and particle size. Table 1
summarizes bead properties. It also shows the log mean diameter
(LMD) values and the span [defined as d50/(d90 – d10)]. The sur-
face area per unit volume was normalized with the value of beads
B2 for comparison. Note that the beads B1 provide lowest surface
area, whereas B3 have the highest surface area among those stud-
ied. It is expected that the surface area of the beads will largely
govern the rheological properties of the suspension, particularly at
high concentrations. Scanning electron microscopy (SEM) shows
that all forms of bead variations look nominally spherical. Fig. 1
also shows the PSD for the B2 beads.
Bentonite was used as a suspending aid in this study. To help
bentonite exfoliate in water, a small amount of soda ash was
added to the formulation. Local tap water was used as a water
source. Three different concentrations of Bentonite were used—
base concentration, 2X the base value, and 3X the base value.
Methods. The liquid glass-bubble additive slurries were prepared
by first premixing the base fluid, consisting of water, a predeter-
mined amount of soda ash, and bentonite in a WaringV R blender
(Maxson et al. 2016). This base solution was then aged at least 24
hours for the bentonite to exfoliate. Then, Glass Bubbles were
slowly added to this base fluid until there was 20% of the Glass Bub-
bles by volume in the base fluid. The mixing speed was kept at less
than 3,000 rev/min to avoid any accidental crushing of the beads.
After mixing, a FannV R 35 viscometer equipped with an F1
spring was used with an FYSA as well as a bob-and-sleeve attach-
ment to collect the rheology data of the base fluid. FYSA is a pre-
ferred method of measuring the volume average-flow response of
the material, particularly when the formulation is heavily loaded
with particulates (Gordon et al. 2007). Fig. 2 illustrates the geom-
etry of the device. This device is akin to vane geometry, and is
highly suited for very thick materials. The details of using FYSA
attachment can be found elsewhere (Johnson and Morgan 2003;
Gordon et al. 2007).
With the FYSA, FannV R 35 dial readings of the 20% Glass
Bubbles by volume liquid additive were obtained and recorded at
3, 6, 100, 200, and 300 rev/min. The procedure was repeated with
increasingly higher amounts of Glass Bubbles added to the same
mix to reach 30, 40, 50, 52.5, 55, 57.5, and 60%, and, in some
cases, 70% of Glass Bubbles by volume of the total amount of liq-
uid. As more beads were added, it became important to ensure
that the formulation was properly mixed and a homogeneous mix-
ture was obtained.
After additional Glass Bubbles were added to the base fluid to
reach the next percentage of bubbles in the total liquid additive,
the FYSA attachments were used on the viscometer to collect the
effective-viscosity values. This method was used to characterize
the different beads (B1, B2, B3, and B4) used in this study.
Suspending-aid (bentonite) concentration was then doubled
(and then tripled), and the procedure was repeated.
To convert the rev/min and dial reading data to shear rate and
stress, the following relations were applied:

Frequency (Compatible) and Undersize

Cumulative Volume (%)
Volume Density (%)

15.0 100.0

10.0
50.0
5.0

0.0 0.0
0.01 0.1 1.0 10.0 100.0 1000.0 10000.0
Size Classes (µm)
(Frequency) - (37) average of 9828 (Undersize) - (37) average of 9828

Fig. 1—PSD for B2 beads. There are 37 bins in the smoothed histogram as indicated in the legend.

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 J181347 DOI: 10.2118/181347-PA Date: 31-May-17
Fig. 2—Image of FYSA attachment to the FannV R 35 viscometer.
FYSA is designed to provide a volume-averaged viscosity of
the formulation, and is preferred to conventional bob and
sleeve for heavily particulated systems as well as foams.
c_ ¼ K1  rev=min ðunits of 1=secÞ
. . . . . . . . . . . . . . ð1Þ
s ¼ K2  DialReadðunits of PaÞ;
where K1 and K2 are constants that depend on the geometry of the
measuring rotor/bob combination and the response spring con-
stant of the equipment. For the FYSA attachment on the FannV R
35 instrument used in this study, which was equipped with F1
springs, K1 ¼ 0:352 and K2 ¼ 0:956.
Fig. 3 presents typical volume-averaged viscosity curves. Note
that the values reported here are termed as volume-averaged vis-
cosity because, with the FYSA, pure viscometric flow is not
achieved; rather, mixing volume is the control element. This is
akin to the work by Metzner and Otto (1957) to obtain the rela-
tionship between impeller speeds and shear rate during mixing. In
this work, the words viscosity and shear rate should be read as
volume-averaged viscosity and volume-averaged shear rate. Note
that similar devices have been used to characterize flow behavior
of proppant-laden fluids (Harris et al. 2005; Harris and Heath
2009; Loveless et al. 2011; Singh et al. 2015a).
The data shown here are for volume fraction of beads varying
from 30 to 70%. The viscosity increases as more beads are mixed
into the formulation. For low amounts of beads (up to approxi-
mately 40%), the dial readings were small, because the formula-
tion is not very thick and the torque signal is very weak. Thus, the
apparent shear thickening at the lowest concentration is not
expected to be physical, and is probably caused by the limitations
1,000
Viscosity 5 minutes
Stress 5 minutes
Viscosity 24 hours
Stress 24 hours
100
Viscosity (cp)
10
1 0.1
0.1 1 10 100
Strain Rate (1/sec)
Fig. 4—Measured rheological curves for base bentonite solu-
tion after 5 minutes of mixing and then after 24 hours.
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100
FYSA; Beads B2
Volume Averaged Viscosity (Pa·s)
10 30%
40%
50%
55%
1
60%
70%
0.1
0.01
1 10 100 1,000
Volume Averaged Shear Rate (1/sec)
Fig. 3—Volume-averaged viscosity as a function of shear rate
for B2 beads with base concentration of bentonite. Bead con-
centration varies from 30 to 70% by volume. Similar results
were obtained for other beads and at higher amounts of sus-
pending aid.
of the viscometer. At the higher concentrations (generally beyond
60%), the formulation was thixotropic in nature. For most of the
analysis in the rest of this work, the bead concentration is re-
stricted to a range of 40 to 60% by volume.
The base-suspending fluid containing bentonite in fresh (tap)
water with small amounts of soda ash was characterized with a
Haake RS150 rheometer, because it was too thin to be character-
ized with a FannV R 35 instrument.
Fig. 4 presents the rheological curves for the base bentonite
solution in water containing a small amount of soda ash. Blue
squares were collected after approximately 5 minutes of mixing
the formulation, and green diamonds were collected 24 hours
later. Filled symbols denote viscosity, whereas open symbols are
measured stress values. The bentonite solution shows highly
shear-thinning behavior. As shown in Fig. 4, no appreciable
change in the rheology was observed, even after 24 hours in the
solution. Primarily, this was attributed to the fact that these solu-
tions were very dilute in bentonite concentration. The key observ-
able difference between 5-minute and 24-hour data is the
reduction in hysteresis after the solution had more time to exfoli-
ate. It is known that the bentonite-exfoliation process may take a
few days to complete (Luckham and Rossi 1999; Abu-Jdayil
2011; Caenn et al. 2011).
Data Analysis and Observations
Effect of Beads Concentration. The first step in understanding
100 the flow behavior of these formulations was to quantify the shear-
thinning and yield-stress (if any) aspects. For each formulation,
power-law, Bingham plastic, HB, Casson, and generalized HB
(GHB) models were fitted. For details of the GHB model, refer to
Ofoli et al. (1987) and Becker et al. (2003). In almost all the
Shear Stress (Pa)
10 cases, one was able to reasonably fit the data with any of these
equations if one based the judgment on R2 value of the fit alone,
with typical value of R2>0.99. It proved to be useful to plot appa-
rent viscosity as a function of stress on a log-log plot to determine
1
the models that better described the experiment.
For example, in Fig. 5, the experimentally measured values
along with the model fits to the data are shown on a log-log scale.
In this case, the Bingham plastic overpredicts viscosity (and the
yield stress) at low stresses, whereas the power law underpredicts
the data. HB and the various forms of GHB fit the data more
1,000 closely. In comparison, the R2 value for the Bingham-plastic
model is 0.9974; for power law, it is 0.9995; and, for HB and
GHB, it is 1.00. The GHB-2 model in Fig. 5 refers to the Casson
equation. In the figure, there are multiple fit lines for GHB-4 and
HB. Because these are nonlinear model fits to the data, the fitting
3
 J181347 DOI: 10.2118/181347-PA Date: 31-May-17 Stage: Page: 4 Total Pages: 10

1 In Figs. 6 and 7, the power-law exponents and the yield stress

of the fits are shown as a function of the beads concentration,
0.8 Experiment value
Power
respectively. From the results, it is apparent that the model param-
eters are quite noisy. Exponent as determined by the HB model is
Log (stres/strain rate, τ/γ )

0.6 Bingham plastic

GHB-2 mostly stable and remains between 0.8 and 1.0, whereas that for
0.4 GHB-3
GHB-4 (HB init)
the GHB model varies from 0.2 to approximately 1.0. When the
0.2 GHB-4 (GHB-3 init) exponent equals unity, both the models reduce to Bingham plas-
HB (GHB-2 init) tic. In general, the power law exponent increases as the concentra-
0 HB (BP init) tion is increased. Thus, it seems that the formulation’s flow
behavior tends toward Bingham plastic at higher concentrations.
–0.2
From Fig. 7, one may conclude that the yield stress generally
–0.4 increases as bead concentration is increased. In fact, for most of
the formulations, the yield stress is practically nonexistent less
–0.6 than 55% bead concentration in the formulations.
–1 –0.5 0 0.5 1 1.5 2
To determine whether the yield stress as determined by the
Log (stress)
model fits is practically relevant, a dimensionless quantity was
Fig. 5—Plot of viscosity and the stress on a log scale for B2
defined as a yield-stress number, which quantifies the signal/noise
beads formulation with 60% beads. ratio in the measurements:
s0
YnHB ¼ ; . . . . . . . . . . . . . . . . . . . . . . . . ð3Þ
algorithm needs an initial guess value, which is indicated in the l1 min½ð_c Þn 
parenthesis. For example, GHB-4 (HB init) implies that the initial
s0
guess values used were the HB parameters. YnGHB-3 ¼ ; . . . . . . . . . . . . . . . . . . . . . . ð4Þ
The GHB model can be written as l1 min½ð_c Þ
 m  m  
s s0 l1 c_ n where min½ð_c Þ refers to the minimum shear rate achieved in the
¼ þ ; . . . . . . . . . . . . . . . . . ð2Þ measurements, which is 1.05 1/sec in this study. Eq. 3 is for the
sref sref sref
HB fluids, whereas Eq. 4 is for the GHB model.
where sref ¼ 47.88 Pa (¼1 lbf/ft2), s is the stress, s0 is the yield Yn is a ratio of the yield stress and the viscous stress in the
stress, l1 is a parameter governing infinite shear viscosity, c_ is measurements. A very small value of Yn indicates that the yield
the shear rate, and m and n are exponents. stress estimated is very small compared with the total stress meas-
The model referred to as GHB-3 is the resultant model when ured by the equipment whereas a large value indicates that the
the exponents m and n take on the same value. The Casson model equipment signal was dominated by the yield stress. In other
(or GHB-2) is obtained when m ¼ n ¼ 0.5. words, values of Yn, which are of the order of unity [O(1)] or
In general, it was determined that the HB and GHB-3 models greater, signify that the estimated yield-stress contribution to the
described the flow behavior most appropriately. signal is significant and that its value is representative of the

1.2 1.2
B1
1.0 1.0 B2
B3
0.8 0.8
Exponent

Exponent

B4
0.6 0.6
B1
0.4 B2 0.4
B3
0.2 0.2
B4
0 0
45 50 55 60 65 70 75 45 50 55 60 65 70 75
Concentration of Beads Concentration of Beads

Fig. 6—Exponents as a function of the concentration of beads (vol%), determined by HB (left) and GHB-3 (right) models for the
four different beads in the formulation.

40 40
B1 B1
35 35
B2 B2
Yield Stress (lbf/ft 2)

Yield Stress (lbf/ft 2)

30 B3 30 B3
25 B4 25 B4
20 20
15 15
10 10
5 5
0 0
45 50 55 60 65 70 75 45 50 55 60 65 70 75
Concentration of Beads Concentration of Beads

Fig. 7—Yield stress as a function of concentration of beads (vol%), determined by HB (left) and GHB-3 (right) models for the four
different beads in the formulation.

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100 100

Yield Stress Number

Yield Stress Number

10 10

1 1
B1 B1
B2 B2
0.1 0.1
B3 B3
B4 B4
0.01 0.01
45 50 55 60 65 70 75 45 50 55 60 65 70 75
Concentration of Beads Concentration of Beads

Fig. 8—Yield-stress number as a function of bead concentration (vol%) determined by HB (left) and GHB-3 (right) models for the
four different beads in the formulation.

measurement. On the other hand, Yn much lower than O(1) indi-
cates that the estimated yield-stress signal is relatively very small,
and its reported value may not be very reliable. Note that this defi-
nition of the yield-stress number is very similar to the Bingham
number (Singh and Denn 2008).
Fig. 8 shows the values of Yn for both HB and GHB fits as
functions of bead concentration. In general, one can observe that
the Yn increases as the formulations become highly concentrated.
At the lower concentrations, the estimated value of yield stress
seems to be insignificant except for the case of B3 beads with HB
model. Note that B3 beads have the highest surface area among
the beads (Table 1) considered, and it is possible that this parame-
ter contributes toward a significant yield stress of the formulation.
B4 beads have the second-highest surface area, and the yield
stress seems to become significant at approximately 52.5% bead
concentration for these beads (for HB model), providing addi-
tional evidence to support the hypothesis. B1 beads with the low-
est surface area do not exhibit significant yield stress until 60%
concentration. These observations are similar to those made for
suspensions in Newtonian fluid because the yield stress increases
with a decrease in the particle size (or an increase in surface area
per unit volume) (Mueller et al. 2010)
From Figs. 6 through 8, it can be noted that the shear-thinning
exponents obtained with HB fits are within a narrow range of
0.8–1.0, and the estimated yield stress at lower concentration
seems to be more significant compared with the GHB-3 model.
Thus, it concluded that the HB model might be more suitable to
describe the flow behavior of these formulations.
Fig. 9 summarizes the shear-thinning exponents obtained with
the HB model for the formulations with different amounts of ben-
tonite. All the shear-thinning exponent values band together in the
range from 0.8 to 1.0, corroborating the earlier conclusion that
these formulations are close to Bingham plastic in terms of the value
of the exponent. Also, it can be noted that the amount of bentonite is
not contributing significantly to the value of exponent observed for
the suspending-aid concentrations explored in this work.
Fig. 10 is a plot of plastic viscosity (or the “consistency” term)
of the HB model with the concentration of beads for various
amounts of bentonite. Open symbols are for B3 beads and closed
symbols for B2 beads. In general, increasing the bead concentra-
tion increases the net-apparent viscosity of the formulation, and
hence, its plastic viscosity. Increasing bentonite concentration
also results in increasing the plastic viscosity. In particular, B3
beads, which have higher surface area compared with B2 beads,
show higher values of plastic viscosity.
Fig. 11 shows the yield stress as a function of bead concentra-
tion. Open symbols represent B3 beads, and closed symbols are
for B2 beads. Again, yield stress increases as a function of the
amount of beads in the formulation. In addition, B3 beads have
higher estimated yield stress compared with the B2 beads. We at-
tribute this to the fact that the B3 beads have higher surface area
per unit volume.
Similar effects of particle size or surface area on the rheology
have been reported in various systems, including dark chocolate
(Afoakwa et al. 2008), coal slurries (Boylu et al. 2004), and poly-
ethylene composites (Joseph et al. 2002).

Effects of Increasing Bentonite Concentration. For B2 and B3 Rheological Modeling

beads, the bentonite concentration in the formulation was
increased to twice and then three times the initial formulation and In the preceding section, it was concluded that an HB form cap-
the rheological characterization was repeated as a function of tures shear-dependent behavior of the formulation. In this section,
bead concentration.
1800
B2; 1X B3; 1X
1.2 1600
B2; 2X B3; 2X
1400 B3; 3X B2; 3X
1.0 1200
μ∞ (cp)

1000
0.8
Exponent

800
0.6 600
400
0.4
B3; 1X B2; 1X B3; 2X 200
0.2 B2; 2DX B3; 3X B2; 3X 0
45 50 55 60 65
0 Concentration of Beads
45 50 55 60 65
Concentration of Beads Fig. 10—Plastic-viscosity term obtained with an HB model as a
function of bead concentration for different amounts of benton-
Fig. 9—Shear-thinning exponent obtained with HB fit for formu- ite concentration in the formulation. Open symbols are B3
lations with varying amounts of bentonite concentration for B2 beads, and closed symbols are B2 beads. The x-axis is in vol-
and B3 beads. The x-axis is in volume (%). ume (%).

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12 f ðCc Þ ¼ A0 þ A1 Cc ; . . . . . . . . . . . . . . . . . . . . . . . . . .ð6Þ
B2; 1X B3; 1X
10 B2; 2X B3; 2X
where A0 and A1 are the two constants to be determined from the
B2; 3X B3; 3X experimental data.
τ0 (lbf/100 ft2)

8 Following Krieger and Dougherty (1959), the following is

proposed:
6  
u a
gðuÞ ¼ 1  ; . . . . . . . . . . . . . . . . . . . . . . . . . ð7Þ
4 um

2 where um is the maximum possible volume fraction of the beads

0 In Fig. 12, apparent viscosity at the volume-averaged shear
45 50 55
Concentration of Beads
Fig. 11—Yield stress obtained with an HB model as a function
of bead concentration (vol%) for B2 and B3 beads. Bentonite
concentration is varied from the base formulation to twice and
three times its value. Open symbols are B3 beads, and closed
symbols are B2 beads.
a model is developed to capture the dependence of the observed
apparent viscosity on the formulation of the suspension. Specifi-
cally, a functional form of dependence on bentonite and beads
concentration is proposed. In addition, a dependence on the bead
PSD is captured with a term dependent on the surface area per
unit volume of the various beads considered.
Typical shear rate experienced by the slurry in the field opera-
tions is 25–40 sec1. For example, a typical scenario of pump-
ing liquefied beads may entail pumping it through a 3-in. hose at
0.25 bbl/min giving effective shear rate 22.9 1/sec. Thus, it was
found appropriate to develop the model for shear rate of 35
sec1 accessible in the Fann 35 viscometer with an FYSA attach-
ment. The proposed model to capture the effective viscosity at
35 sec1 is
l35 ¼ l035 f ðCc ÞgðuÞsðdÞ; . . . . . . . . . . . . . . . . . . . . . ð5Þ
where l035 is a constant, f ðCc Þ captures the dependence on clay
concentration (bentonite), gðuÞ represents the dependence on the
bead concentration, and sðdÞ captures the effect of surface area
offered by particles on per unit volume basis. HB model, by use
of Eq. 2 with appropriate values of yield stress, plastic viscosity
and the exponent can be used to extend this model to other shear
rates of interest.
Because the base solution is relatively dilute in terms of clay,
after Taylor’s expansion, a liner dependence of the viscosity on
the clay concentration is proposed, or
and a is the exponent to be determined from the experimental data.
60 65 rate of 35 sec1 is shown as a function of bead concentration
for both the B2 and B3 beads. The plot on the left is for B2 beads,
and the plot on the right is for B3 beads. The plots clearly show
that the viscosity increases sharply with bead concentration. In
addition, in comparing the two plots, it can be observed that the
Sample B3 has much higher viscosity compared with the corre-
sponding sample of B2. This is because of a much higher surface
area per unit volume (or smaller net particle size) in Sample B3.
At such high bead concentration, the shear response of the sample
is expected to be dominated by the resistance of beads sliding past
each other. If one assumed body-centered cubic packing of spheri-
cal particles, the average minimum distance between the surfaces
of two neighboring particles will be 0.04 times the particle size
or roughly 1 to 2 mm for a 40-mm particle. The lines in Fig. 12 are
power-law fits to the viscosity data.
Effect of Bentonite Concentration. Fig. 13 shows that the appa-
rent viscosity at the shear rate of 35 sec1 increases almost line-
arly with the clay concentration for both the B2 and B3 samples,
respectively, except for the 60% concentration of B3 beads. The
plot on the left is for B2 beads and the plot on the right is for B3
beads. The concentration of the beads varies from 50% (blue dia-
monds) to 60% (red squares). This corroborates the expectation
from Eq. 6 that the net dependence of viscosity on bentonite con-
centration can be captured by a linear relationship.
In addition, as the bead concentration is increased, the viscos-
ity is more sensitive to the clay concentration, indicated by the
increase in the slope of linear fits to the data.
Effect of Bead Concentration. The Krieger-Dougherty form of
viscosity (Eq. 7) implies that viscosity will essentially tend to in-
finity as the maximum packing fraction of the beads is
1
approached, or  0 as u  um .
l
In Fig. 14, the reciprocal of viscosity as a function of the vol-
ume fraction of the beads is shown. The left figure is for B2 beads,

1.4 2.5

1.2 1X 1X y = 358.04x 10.181

2X y = 36.114x 6.818 2 2X R 2 = 0.9952
3X R 2 = 0.9738
Viscosity at 35 sec–1

Viscosity at 35 sec–1

1.0 3X

0.8 1.5

0.6
1

0.4
y = 156.02x 9.7568
y = 9.237x 6.0018 0.5
R 2 = 0.9947
0.2 R 2 = 0.9741

0 0
0.48 0.5 0.52 0.54 0.56 0.58 0.6 0.62 0.48 0.5 0.52 0.54 0.56 0.58 0.6 0.62
Beads Volume Fraction Beads Volume Fraction

Fig. 12—Viscosity at shear rate of 35 sec21 (Pas) as a function of the concentration of B2 (left) and B3 (right) beads. Green trian-
gles are at the highest bentonite concentration, whereas blue diamonds are at the lowest bentonite concentration. The lines are a
power-law fit to the data.

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 J181347 DOI: 10.2118/181347-PA Date: 31-May-17 Stage: Page: 7 Total Pages: 10

1.4 2.5

1.2

Viscosity at 35 sec–1

Viscosity at 35 sec–1
60% y = 0.3666x + 0.0453 2 60%
57.5% R 2 = 0.9887 57.5%
1.0 y = 0.4617x + 0.507
55% 55% R 2 = 0.772
52.5% 1.5 52.5%
0.8 y = 0.258x + 0.0453
50%
50% R 2 = 0.9774

0.6 y = 0.163x + 0.0543

1
R 2 = 0.9231
y = 0.0951x + 0.0996
0.4 R 2 = 0.8547

0.5
0.2 y = 0.1086x + 0.0091
y = 0.0679x + 0.1177
R 2 = 0.9231
0 0 R 2 = 0.9868
0 0.5 1 1.5 2 2.5 3 3.5 0 0.5 1 1.5 2 2.5 3 3.5

Bentonite Bentonite

Fig. 13—Viscosity at the shear rate of 35 sec21 (Pas) as a function of the concentration of bentonite for B2 (left) and B3 (right)
beads for various bead concentration in the formulation. Lines are a linear fit to the data. Note that the bentonite concentration
has been scaled with the base-blend concentration.

and the right figure is for B3 beads. Blue diamonds are at base  1
u
concentration of bentonite, red squares are at the intermediate, l35  1 : ........................ ð8Þ
um
and the green triangles are at the highest concentration of benton-
ite. Solid lines are a linear fit to the data.
One estimate of the maximum packing fraction of beads can Before proceeding further, the data set was reduced to under-
be made by extrapolating the data to the zero intercept on the stand how well the model could predict the linear dependence of
x-axis. By the extrapolation of the linear fits, it can be observed viscosity on the bentonite concentration and Krieger-Dougherty
that the maximum packing fraction for the B2 beads is approxi- dependence on the beads concentration. In particular, to remove
mately um  0:63  0:64 and is 0.62 for B3 beads. Note that any dependence on the bead volume fraction from the data, the
B3 has a smaller span or narrower PSD (Table 1). This probably following relationship for reduced viscosity was defined:
explains the slightly smaller value for the maximum packing frac-
tion for the B3 beads, as the wider the distribution, the higher the  
u
packing efficiency. In comparison, random close packing of lr ¼ l35 1  : . . . . . . . . . . . . . . . . . . . . . . . . ð9Þ
um
spheres is close to 0.64. Van der Werff and De Kruif (1989) have
confirmed a maximum packing fraction of 0.63 for a system of
submicron sterically stabilized silica dispersions. For a self-sus- Fig. 16 shows the reduced viscosity as a function of the ben-
pended system of Brownian particles, the estimate of maximum tonite concentration. Blue circles represent B3 beads, and red
packing fraction at which the transport quantities diverge is close squares are for the B2 beads. Note that most of the data for a
to 0.5 (Singh et al. 2015a, 2015b). given bead collapses together, indicating that the bead-concentra-
Using the calculated um ; the exponent in the Krieger-Dough- tion dependence is captured fairly well by the Krieger-Dougherty
erty form can  be estimated.
 In Fig. 15, viscosity is shown as a form proposed. A straight-line fit to the reduced viscosity con-
u firms that the dependence on the clay concentration is linear. In
function of 1  on a linear scale. By using a power law fit
um addition, the two linear fits are almost parallel to each other, with
(or a linear fit on a log-log scale) to the data, it can be observed B3 having a higher reduced viscosity compared with B2. These
that, for B2 beads, the exponent is between –0.85 and –1.0, differences can be attributed to the differences in the bead proper-
whereas, for B3 beads, the exponent varies between –0.97 and ties. Because both the beads are chemically similar (they are both
–1.01. For the sake of simplicity, the exponent was set equal to made of very similar glass compositions) and have similar sphe-
negative unity for the remainder of the work. Thus, ricity, it can be concluded that the differences between the two

8 6.0

y = –43.73x + 26.75 1X
7
5.0 R 2 = 0.95
2X
1/Viscosity at 35 sec–1

1/Viscosity at 35 sec–1

6
3X
4.0
5

4 3.0
y = –39.78x + 25.03
y = –46.64x + 29.94
R 2 = 0.99
3 R 2 = 0.90
2.0
2 1X y = –32.29x + 19.93
y = –25.73x + 15.69
2X R 2 = 0.95 R 2 = 0.95
1 1.0
y = –20.88x + 13.30
3X
R 2 = 0.99
0
0.0
0.48 0.53 0.58 0.63 0.48 0.53 0.58 0.63
Beads Volume Fraction Beads Volume Fraction

Fig. 14—Inverse of viscosity (1/Pas) at the shear rate of 35 sec21 as a function of the bead concentration showing the linear rela-
tionship between the two. B2 beads are on the left, and B3 beads are on the right.

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 J181347 DOI: 10.2118/181347-PA Date: 31-May-17 Stage: Page: 8 Total Pages: 10

1.4 1.6
1X 1X
1.2 2X 1.4
2X
3X
Viscosity at 35 sec–1

Viscosity at 35 sec–1
1.2 3X
1
1
0.8 y = 0.0245x –1.69
0.8 R 2 = 0.997
y = 0.0839x –0.94
0.6 R 2 = 0.9799
0.6
0.4
0.4

0.2 y = 0.0467x –0.803 y = 0.0169x –1.586

0.2
R 2 = 0.9227 R 2 = 0.9816
0 0
0.000 0.050 0.100 0.150 0.200 0.250 0.000 0.050 0.100 0.150 0.200 0.250
1–ϕ/ϕm 1–ϕ/ϕm

Fig. 15—Plot of viscosity (Pas) at the shear rate of 35 sec21 as a function of the beads concentration showing the validity of Krieger-
Dougherty form for viscosity. B2 beads are on the left, and B3 beads are on the right. The exponent is found to be close to unity.

data sets can be attributed to the different surface area (or particle squares are for B2 beads. Within the experimental variability,
size) offered by the two. both the data sets for the beads overlap, indicating that the model
Earlier in this section, it was proposed that the contribution properly accounts for the differences in the beads by means of the
attributed to the surface area might be captured by a multiplica- surface-area term. This dependence on specific surface area is
tive factor. Under highly concentrated conditions, the response of similar to the dependence of yield stress on surface area of alu-
the fluid when sheared will be dominated by the beads flowing mina particles suspended in aqueous media as reported by Zhou
past each other. Thus, the response of the fluid being sheared et al. (1999).
between the beads plays an important role in determining the
overall flow behavior of the formulation. In other words, the fol- Conclusions
lowing relationship was proposed:
In this work, the liquid formulation of hollow glass beads has been
    developed, and its flow behavior is characterized. Extensive FannV R
u 1 SA c
l35 ¼ l035 ðA0 þ A1 Cc Þ 1  : . . . . . . . . ð10Þ 35 instrument rheological data by use of the FYSA rotor and sleeve
um SA0 at various concentrations of beads and suspending aid (bentonite)
In particular, this work quantified further the surface-area were collected for four types of beads. It was shown that the analy-
1 sis of the FannVR 35 instrument rev/min Dial read data was an im-

exponent as c ¼ ; where SA is the specific surface area of the portant step in understanding rheology and how relying on R2
2 values could result in suboptimal characterization. Instead, a log-
beads and SA0 is the surface area per unit volume offered by B2
beads. Updated reduced viscosity is defined by log plot of viscosity with shear stress should be used.
It was found that the formulation behavior is close to power
 
u law for low concentrations (close to 50%), and tends to Bing-
lr2 ¼ l35 1  d; . . . . . . . . . . . . . . . . . . . . . ð11Þ ham plastic at the highest concentrations studied (60% and
um
greater). In general, the HB model captures the overall behavior
sffiffiffiffiffiffiffiffiffiffiffiffiffiffi
ffi with shear-thinning exponent varying from 0.8 to 1.0.
SA In addition, a criterion was developed for determining the sig-
where d ¼ .
SA0 nificance of estimated yield stress compared with the net stress
In Fig. 17, this updated reduced viscosity is shown as a func- measured by the equipment.
tion of bentonite concentration. Blue circles are B3 beads, and red

0.10
0.14
Reduced Viscosity at 35 sec–1

0.09
y = 0.0215x + 0.0067
Reduced Viscosity at 35 sec–1

0.12 0.08
R 2 = 0.8949
B2 0.07
0.10 B3
y = 0.0215x + 0.0295 0.06
R 2 = 0.6018 0.05
0.08
0.04
0.06 0.03 y = 0.0149x + 0.0204
R 2 = 0.6018
0.02
0.04
y = 0.0215x + 0.0067 0.01
R 2 = 0.8949
0.02 0.00
0 0.5 1 1.5 2 2.5 3 3.5 4
0.00 Bentonite
0 0.5 1 1.5 2 2.5 3 3.5 4
Bentonite Fig. 17—Reduced viscosity (Eq. 11) taking into account the par-
ticle concentration and the differences in the surface area of
Fig. 16—Reduced viscosity (Eq. 9) as a function of bentonite the two beads is shown as a function of bentonite concentra-
concentration (scaled with respect to the base concentration). tion (scaled with respect to the base concentration). Blue
Blue circles are for B3 beads, and red squares are for B2 beads. circles are for beads B3, and red squares are for beads B2.

8 2017 SPE Journal

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 J181347 DOI: 10.2118/181347-PA Date: 31-May-17
Increasing the concentration of beads led to increased slurry
viscosity and enhanced yield stress for a given formulation. The
surface area of the beads plays a significant role in viscosifying
the solution. In addition, it was confirmed that the broader the dis-
tribution of beads, the more efficiently they pack, and the maxi-
mum packing fraction as estimated was increased. Overall, the
Krieger-Dougherty relationship adequately captured the flow
behavior of these formulations.
Bentonite concentration also enhanced the viscosity of the for-
mulation. It was found that the viscosity depends linearly on the
bentonite concentration.
A comprehensive model that elucidates and combines all these
effects was developed, and is shown to capture the flow behavior
reasonably well.
Nomenclature
A0 ¼ constant, unitless
A1 ¼ constant, unitless
Cc ¼ p normalized
ffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi bentonite concentration, dimensionless
d ¼ SA=SA0 , dimensionless
K1 ¼ FYSA constant, min/s/rev
K2 ¼ FYSA constant, Pa/degree
m ¼ constant exponent in GHB equation (Eq. 2)
n ¼ constant exponent in GHB equation (Eq. 2)
SA ¼ surface area per unit volume, 1/m
SA0 ¼ surface area per unit volume of beads B2, 1/m
a ¼ constant, unitless
c ¼ constant, unitless
c_ ¼ shear rate, 1/sec
l ¼ volume averaged viscosity, Pas
lr ¼ reduced viscosity, Pas
l35 ¼ viscosity at shear rate of 35 s1
l035 ¼ constant, Pas
l1 ¼ plastic viscosity or “consistency factor,” Pas
s ¼ stress, Pa
sref ¼ reference stress value, 47.88 Pa
s0 ¼ yield stress, Pa
u ¼ volume fraction of glass beads
um ¼ maximum volume fraction of glass beads
Acknowledgments
The authors acknowledge Halliburton for permission to pursue
and publish this work.
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Simone E. A. Lumsden was an associate scientist in the
Cement Research and Development Department at Hallibur-
ton for 2 years. Her research interests include organometallic
10
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Stage: Page: 10 Total Pages: 10
chemistry and hydrogenase enzyme chemistry. Lumsden has
authored one other technical paper. She holds a BS degree in
chemistry from the University of Texas at Austin.
John P. Singh is a principal technical professional at Halliburton
Energy Services (HES). His interests include rheology, multi-
phase flows, and process modeling. At HES, Singh has been
applying chemical-engineering principles to process and
product research and development (R&D) for the last 2 years.
He has authored 12 papers, 13 patent applications, and multi-
ple trade reports. Singh holds a B. Tech degree in chemical
engineering from IIT-Delhi, India, and MS and PhD degrees
from City College of New York.
Ronnie G. Morgan is chief technical adviser at HES. He has
been with the company for 21 years. Morgan’s interests
include rheology and non-Newtonian fluid mechanics related
to cementing oil and gas wells. He holds BS and MS degrees in
agricultural engineering from Oklahoma State University and a
PhD degree in agricultural engineering from Texas A&M
University.
Greg Hundt is a discipline lead in the Halliburton Cementing
Applied Sciences Group. His professional interests include or-
ganic synthesis and materials characterization. Hundt has
authored or coauthored five technical papers and holds
three patents. He holds a PhD degree in chemistry from the
University of Texas at Dallas.
2017 SPE Journal