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IPTC 14952

An Experimental Investigation on use of Nanoparticles as Fluid Loss


Additives in a Surfactant – Polymer Based Drilling Fluid
Jayanth T. Srivatsa, Malgorzata B. Ziaja, Texas Tech University in Lubbock

Copyright 2011, International Petroleum Technology Conference

This paper was prepared for presentation at the International Petroleum Technology Conference held in Bangkok, Thailand, 7–9 February 2012.

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Abstract

As we approach an age of deeper discoveries in hostile environments, we need to either improve on existing drilling fluids or
design new ones in order to meet the technological demands for success. The filtrate invasion is the most critical parameter
that may cause a wellbore failure if not properly controlled. Also, the filtrate induced formation damage and problems with
filter cake removal adversely affect the well productivity or injectivity.

The literature survey reveals the advantages of polymer, surfactant and Nanoparticles systems independently and also
combination of two of these. A study is necessary to see the effect and advantages of combining all three systems together i.e.
a Polymer-Surfactant-Nanoparticles system and to measure the rheological and fluid loss characteristics of the complex
combined drilling fluid system. An attempt to study the same has been made in paper. Therefore, in this paper the authors
present the results of testing the rheological properties and the API filtrate loss of a Bio-Polymer and Surfactant blend system
with addition of Nanoparticles and compare the fluid loss reduction by using Nanoparticles as fluid loss additive with an
industry standard polymer-based fluid loss additive

The objective of this research was to study the effectiveness of a Bio Polymer - Surfactant fluid blends, containing
Nanoparticles as fluid loss additives in reducing the filtrate losses to the formation by forming a thin, non-erodible filter cake.

Laboratory experiments were carried out for the different combination of polymer and surfactant with varying concentrations
to find the optimum of fluid performance. The laboratory measurements included measuring mud weight, pH, viscosity, gel
strength, standard API filter test and High Temperature High Pressure (HTHP) test using Permeability Plugging Apparatus.

Presented results show that sized silica nanoparticles can be used instead of sized calcium carbonates which are a very
effective inorganic bridging agent, however, difficult to maintain. The polymer - surfactant blend is better in rheological
properties as well fluid loss properties than a Bio-Polymer based fluid or Surfactant based fluid. It captures the merits of both
fluid systems. The nanoparticles play an important role in reducing the fluid loss of the individual fluid systems. Also, the
nanoparticles based Polymer-Surfactant blend is a good solution for solids free reservoir drill in fluids for horizontal shale
drilling applications. The nanoparticles is most effective for shale drilling application as it can penetrate the pores of the
shale and act as a bridging material and causing wellbore strengthening.

Introduction

The search for oil and gas has moved out of the “easy-to-get-to” shallow productive pay zones. With the advances in 3-D
seismic technology many new potential reservoirs have been found which are located beneath the old depleted producing
zones. The access to these zones requires drilling through earlier produced zones. The zones which have been producing oil
and gas for many years have depleted reservoir pressures and mud weight balance required to balance reservoir pressures
below the depleted sand may be considerably higher. The problems faced when drilling through these depleted sands are
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primarily differential sticking and loss of returns. The proper addressing of these problems can mean the difference between
successful completion of drilling and loss of the wellbore. Also, the advanced drilling technologies such as multilateral wells
or slim hole drilling require special fluids that minimize pressure losses at the same time maintaining effective cutting
carrying properties and have a non-damaging behavior.

Improved drilling fluids which satisfy both drilling and completion requirements and can be successfully applied for drilling
operations in complex formations or in depleted reservoirs is the need of the hour. However minimizing formation damage is
always the priority in order to optimize production. In order to achieve the same, most of the drilling fluids developed by
major service companies contain Bio-Polymers and soluble sized bridging solids. Reduction of bridging solids concentration
and substituting it with polymeric additives that have stronger shear thinning characteristics and higher temperature stability
is the current challenge facing the industry.
The density adjustments to solid free drilling fluids must be made from high-density brines rather than solids to maintain an
ultra-thin filter cake and a low viscosity profile [1]. Several studies have been carried out on reservoir drill-in or solids free
fluids [2-3] to minimize filtrate-induced damage and to obtain the maximum well conductivity. Oil-based muds can be used
while drilling through troubled sections such as shale where stability is an issue. They have superior temperature stability,
lubricity and hole stabilizing attributes which cannot be matched by water-based muds. But the major disadvantages being
environmental concerns along with high costs and handling issues. Therefore a search for alternate water-based muds with
advantages of Oil-based muds and at the same time being environmentally friendly is required. The search for such muds has
led to use of Bio degradable Polymers and synthetic fluids for drilling and completions.

The aim of this research is to check the fluid loss values when Nanoparticles are used as fluid loss additive. The
improvements in rheological properties are also studied. Nanotechnology is a branch of science and technology where the
size particles between 1 – 100 nm are studied. It can be used to solve a lot of problems associated with drilling engineering.
The Nanoparticles have high area to volume ratio which gives them a high surface area for interaction with surrounding
medium, hence for any application the quantity of nano particles required will be less and hence there is cost advantage when
using Nanoparticles. Here, the applications of Nanoparticles in drilling fluids is mainly to form a thin layer of non-erodible
and impermeable Nanoparticle membrane around the wellbore which prevents common problems like clay swelling, spurt
loss and mud loss due to circulation. These nano-particles can also eliminate use of additives, shale inhibitors, rheology
modifiers and can be very easily removed during clean-up before completion operations.

The literature survey reveals the advantages of polymer, surfactant and Nanoparticles systems independently and also
combination of two of these. A study is necessary to see the effect and advantages of combining all three systems together i.e.
a Polymer-Surfactant-Nanoparticles system and to measure the rheological and fluid loss characteristics of the complex
combined drilling fluid system. An attempt to study the same has been made in paper. Therefore, in this paper the authors
present the results of testing the rheological properties and the API filtrate loss of a Bio-Polymer and Surfactant blend system
with addition of Nanoparticles and compare the fluid loss reduction by using Nanoparticles as fluid loss additive with an
industry standard polymer-based fluid loss additive.

Experimental Setup
The authors studied the rheology of the fluids and fluid loss characteristics at 75° F, 100 psi and 200° F, 1000 psi. The test
results were obtained using the standard viscometer, the API (American Petroleum Institute) Filter press and Particle
Plugging Apparatus (PPA).

The fluid preparation involved various stages and each had to be carried out in particular order for achieving consistent fluid
blends for the results to be reliable. Maintaining pH of the blends was also an important step in preparation of the fluid.

The first step was to prepare the polymer and surfactant blend. The additives were added in reference to sample sizes of 1000
mL. About 1.75 lb/bbl was weighed on a balance and slowly added to blending jar such as Warren blender while taking care,
that vortex formation does not allow air bubbles to get trapped. The polymer is dispersed slowly and Hydrochloric acid was
used to bring down the pH to about 4 or 5 to help polymer disperse uniformly. While the polymer is being dispersed, a 2% by
wt KCl was weighed and added to the sample as an inhibitor. The pH needs to be adjusted back to 10 by using a base. pH
paper was used to measure the pH while preparing the fluids. After about 20 min. of blending the polymer sample was kept
aside for 24 hrs to dehydrate.

The 5% by volume surfactant-based fluid was prepared by adding appropriate amount of VES (Visco Elastic Surfactant) to
2% KCl brine solution. The mixture is blended for about half an hour and set aside for hydration for about 24 hours. After
hydration, an appropriate amount of 5 % VES and polymer are added and blended for about 5 min to prepare the sample of
required concentration of polymer and surfactant. Nanoparticles are added 10% by wt to samples in a slow manner without
causing aggregation.
IPTC 14952 3

The experimental analysis was performed on each of the base fluids initially to understand the nature of fluid loss of Polymer
and Surfactant fluids individually. The laboratory measurements included measuring mud weight, pH, viscosity, gel strength,
standard API filter test and High temperature high pressure (HTHP) test using Particle plugging apparatus (PPA) which are
discussed in the previous test.

The test was then carried out by changing the concentration of Polymer and surfactant with reducing polymer concentration
at each trial. Three trials were carried out for the combination of polymer and surfactant with varying concentrations as listed
below

• 90% of Polymer and 10% of Surfactant


• 70% of Polymer and 30% of Surfactant
• 50% of Polymer and 50% of Surfactant

The trials were stopped at 50% concentration of Surfactant as the fluid loss exceeds the benefits of combined fluid systems or
the polymer fluid systems alone. It is well documented in petroleum and chemical literature that mixtures of anionic
Surfactants and different water-soluble polymers tend to phase separate in saline aqueous solutions when the concentrations
of Surfactants usually exceed 5 – 10 wt% [38].

The next step was to test these fluid systems with addition of Nanoparticles. 10% wt/wt colloidal silica Nanoparticles were
added to the fluids as explained in the previous chapter. 10% wt/wt concentration was chosen based on the background study
[18]. Later, the concentrations of Nanoparticles were increased to 20% and 30% to see the effect of increasing concentrations
of Nanoparticles.

The next set of trials was run on high temperature high pressure apparatus known as particle plugging apparatus. The same
concentrations of polymer and Surfactant blends without addition of Nanoparticles and also with addition of Nanoparticles
were repeated at 1000 psi pressure and 200° F temperatures.

The last set of trials was carried out in order to compare the addition of Nanoparticles as a fluid loss agent with a standard
fluid loss additive available in the industry. The fluid loss additive was a polymer-based additive and not a bridging agent and
hence the testing of the same on HTHP system was not necessary as it would be having the same wall building properties as
the polymer fluid system.

The samples were designated by letters for easy identification. Samples beginning with prefix „a‟ were sample without
addition of Nanoparticles. Samples beginning with prefix „n‟ were samples containing Nanoparticles. Prefix „b‟ designates
the standard fluid loss additive. The sample nomenclature is as listed below.

Sample a1: 1.75 lb/bbl Xanthan gum


Sample a2: 5% v/v Visco elastic surfactant
Sample a3: 90% of 1.75 lb/bbl Xanthan gum and 10% of 5% v/v surfactant
Sample a4: 70% of 1.75 lb/bbl Xanthan gum and 30% of 5% v/v surfactant
Sample a5: 50% of 1.75 lb/bbl Xanthan gum and 50% of 5% v/v surfactant
Sample n1: 1.75 lb/bbl Xanthan gum + 10% wt/wt Nanoparticles
Sample n2: 5% v/v Visco elastic surfactant + 10% wt/wt Nanoparticles
Sample n3: 90% of 1.75 lb/bbl Xanthan gum + 10% of 5% v/v surfactant + 10% wt/wt Nanoparticles
Sample n4: 70% of 1.75 lb/bbl Xanthan gum + 30% of 5% v/v surfactant + 10% wt/wt Nanoparticles
Sample n5: 50% of 1.75 lb/bbl Xanthan gum + 50% of 5% v/v surfactant + 10% wt/wt Nanoparticles
Sample n6: 90% of 1.75 lb/bbl Xanthan gum + 10% of 5% v/v surfactant + 20% wt/wt Nanoparticles
Sample n7: 90% of 1.75 lb/bbl Xanthan gum + 10% of 5% v/v surfactant + 30% wt/wt Nanoparticles
Sample b1: 1.75 lb/bbl Xanthan gum and 1 lb/bbl of Fluid loss additive
Sample b2: 90% of 1.75 lb/bbl Xanthan gum + 10% of 5% v/v surfactant + 1 lb/bbl of fluid loss additive
Sample b3: 70% of 1.75 lb/bbl Xanthan gum + 30% of 5% v/v surfactant + 1 lb/bbl of fluid loss additive
Sample b4: 50% of 1.75 lb/bbl Xanthan gum + 50% of 5% v/v surfactant + 1 lb/bbl of fluid loss additive

Experimental Results

Mud weight and pH measurement

The mud weight of all the samples along with pH measurements is listed in Table A-1. The results shown in Table A-1
clearly indicate that mud weight remains almost constant with all the blends. The addition of nano particles does not
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significantly increase the mud weight. This gives an advantage in selection of Nanoparticles as bridging agent and thereby
reducing the increase of solid concentration in the drilling fluids especially in reservoir drill in fluids used for high angle
wells, horizontal and directional wells.

From Table A-2 it is very clear that even with significant increase in Nanoparticles as a bridging agent, the mud weight
remains fairly constant. The pH was adjusted to be 10 mostly, but a slight variation is due to non-availability of pH meter for
accurate measurements. The measurements were done using a pH paper.

Rheology Measurements

Samples without addition of Nanoparticles

The Fann 35 viscometer was used to measure the shear characteristics of the drilling fluid at six different speeds. The
experiments were conducted at room temperature of 75° F. The 10 s and 10 min gel strength were also measured.

The plot of apparent viscosity and shear rate as show in Fig B-1 indicates that samples a3 and a4 which are a blend of
surfactant and polymer have a better linearity curve at high shear rates than sample a1 with just polymer or a2 with just
surfactant. As the surfactant concentration increases the fluid looses the linearity at high shear rates. This is mainly due to
long chain polymers being randomly entangled when they are at rest, but when set in motion the chains align parallel to the
direction of flow [39]. Blends a3 and a4 is in line with minimum recommended treatment of biopolymer of 1ppb to 2ppb in
most water-based fluids [8]. Biopolymer concentration may be increased for further increase in viscosity. The power law
model is used to characterize the flow behavior of the pseudo-plastic fluids. K is known as the consistency index and n is
known as the flow behavior index. For a Pseudo-plastic fluid; n < 1. Fig B-2 shows the plot of Shear stress v Shear strain.
The curve shape indicates the Pseudo-plastic behavior of the blend. The mixture of polymers surfactant matches the
performance of polymer fluid system.

Samples after treatment with Nanoparticles

The tests are repeated for the same concentrations of polymer and surfactant as listed above, but 10% wt/wt colloidal silica
Nanoparticles are added to the mixture. The Nanoparticles is mainly used as fluid loss agent to plug the pores of the
formation especially shale, however the addition of Nanoparticles caused a better performance of the fluids in shear
conditions.

Fig B-3 indicates blends n3 and n4 match the performance of polymer fluids n1 and also the rheology of the fluids show a
better performance compared to samples prior to treatment of Nanoparticles as shown in Fig B-4.

Performance improvement of blends after addition of Nanoparticles

Fig B-5 shows a plot of sample a1 and a3 with n1 and n3, i.e. polymer fluid with and without addition of Nanoparticles, the
viscosity for sample n1 shows a 30% increase in viscosity at high shear rates than sample a1 and n3 shows a 36% increase as
compared to a3.

By using specific tailor made Nanoparticles the viscosity can be increased significantly then a cross-linked polymer gel
system and also strong 3 dimensional structures are formed [26]. Thus due to atomic scale surface forces playing a dominant
role there is better physio-chemical process acting in nano-materials and nano-based fluids. [15].

A standard polymer-based fluid loss additive (FLA) was used to compare the effectiveness of the nano fluids. The rheology
was tested and as expected it did not make a huge difference as it mainly a polymer-based additive and mainly used for fluid
loss reduction. Figure B-6 shows the readings of fluid systems with standard fluid loss additive. The addition of FLA helps
achieve a linear response to different shear rates but at high shear rate viscosity is better achieved with Nanoparticles.

Samples with Fluid Loss Additive

A standard polymer-based fluid loss additive was used to compare the effectiveness of the nano fluids. The rheology was
tested and as expected it did not make a huge difference as it mainly a polymer-based additive and mainly used for fluid loss
reduction. Figure B-6 shows the readings of fluid systems with FLA. The addition of Bore-plus help achieve a linear
response to different shear rates but at high shear rate viscosity is better achieved with Nanoparticles.
IPTC 14952 5

Effect on rheology addition of higher concentrations of Nanoparticles to nano fluids

The particle concentration in nano fluids was increased to 20% wt/wt and 30% wt/wt from the original 10% wt/wt
concentration. The trials were carried out only one sample i.e. 90% Xanthan fluid + 10% by vol of 5% VES surfactant. The
effect on rheology is shown below in the Table 10 and Fig 7. The addition of additional Nanoparticles created a slight change
in the rheology increasing the linearity of the curve and supports the theory that Nanoparticles behavior is governed by
Nanoparticles grain boundary and surface area / unit mass. Thus, the addition of small concentrations of Nanoparticles is
sufficient to cause significant physio-chemical changes in the system [15].

The above results are only indicative of the colloidal form of Nanoparticles which form “super-miscellar” aggregates.
Complex mixture had a remarkable stability of the hybrid aggregates and the dependence of the sizes on the stability. The
results of rheology may vary with use of different form of Nanoparticles like, crystalline form. Also the rheology of the fluids
might change with different sizes of Nanoparticles. The results are highly dependent on the hydroxyl group (-OH) on the
surface of Nanoparticles which causes Nanoparticles to be agglomerated in an organic solution [29]. The surfactant addition
significantly affects the agglomeration and hence the concentration of surfactant as it increases causes more agglomeration of
the Nanoparticles in organic solution and hence the rheology response of the fluid is lower than higher concentrations of
Surfactants.

Standard API fluid loss tests

The main aim of the study was to investigate the behavior of Nanoparticles as a fluid loss additive. The samples were
subjected to a 100 psi pressure and at 75° F the fluid loss in a standard API filter press and fluid loss across the API filter
paper was measured. The results of these were then compared to fluid loss of the samples with Nanoparticles and also the
samples with fluid loss additive.

The tests were then carried out on a HTHP filter press assembly known as Particle plugging apparatus at 1000 psi pressure
and 200° F. The HTHP assembly used a ceramic disc of 775mD permeability instead of the standard API filter paper. This
disc with a permeability and porosity represents the formation better than filter paper.

API filter press test on samples before addition of Nanoparticles

Figure B-8 shows the fluid loss over a period of 30 min for different samples without Nanoparticles. The spurt losses were
calculated with extrapolating to zero time. The blend of polymer and surfactant has a better fluid loss characteristics
compared to biopolymer. The blend a3 has a fluid loss of 13.1 mL compared to biopolymer a1 which has a fluid loss of 17
mL. This reduced fluid loss may be due to the similarities in the polymer and surfactant molecules, surfactant molecule are
attracted towards the polymer molecules and also induce the formation of micelles. The main attraction forces are
hydrophobic and the presence of oppositely charged particles enhances interaction [12]. A complete flush is observed with
just surfactant as base fluid. The fluid loss of sample a5 is almost equal to that of sample a1. This indicates as the Surfactant
increases the stability of the fluid decreases and does not form a strong bond to reduce the spurt and fluid loss. Thus a
minimum concentration of biopolymer and a limit to surfactant concentration is about 1.57 lb/bbl (90%) and about 10% of
5% VES concentration for optimum results [24].

API filter press test on samples after addition of Nanoparticles

The API fluid loss of the sample saw a decrease in fluid loss over a period of 30 minutes as much as 50%. Figure B-11 shows
a comparison between the samples before and after addition of Nanoparticles. The sample n3 had the best performance of the
samples having the least fluid loss at 7.9 mL; in comparison the sample a3 without addition of Nanoparticles had a fluid loss
of 13.1 mL, a reduction of 40%. Other blends with addition of Nanoparticles had similar characteristics. The blend also had a
lower spurt loss values. The blend a5 with 50% of surfactant and 50% of biopolymer did have similar characteristics of other
blends achieving a lower fluid loss with Nanoparticles compared with non Nanoparticles blend, but since the concentration of
the surfactant was 50% it had the highest fluid loss among the blends and even more than biopolymer fluid alone.

Figures B-12, B-13 and B-14 show the actual mudcake formation after 30 min on a API filter press at 100 psi pressure and
75° F temperature. Figures B12 and B-13 show the mudcake formation with Nanoparticles. The Nanoparticles deposit a fine
layer of particles after the formation of an internal mud cake by the organic polymer. This helps prevent the damage by
polymers invading the formation and causing formation damage. The layer of cake deposited is very thin and comparable to a
cake as caused by using just biopolymer alone. The complex mixture forms very stable hybrid aggregates [31]. Figure B-14
shows a mudcake formation of Surfactant n2 and Nanoparticles combination. The surfactant sample a2 without any addition
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of Nanoparticles had a complete flush, an uncontrolled fluid loss when subjected to filter press assembly. The mudcake
formation as seen from the figure is not as fine and uniform as observed in the other blends, but there was a controlled fluid
loss and not a complete flush. This is due to formation of worm like micelles and pseudo-crosslink characteristics of the
worm like micelles in surfactant systems first associate with end caps which are energetically unfavorable and then this
become junctions for worm like micelles, which enhance the wall building characteristics of the miscellar fluid system [27].

Due to its high surface to volume ratio the particles in the mud cake matrix can easily be removed by traditional cleaning
systems during completion stages. Thus the nano particles can be used as rheology modifiers, fluid loss additives and shale
inhibitors with unparalleled properties for very small concentrations of the particle. Thus the smart fluids based on nano
fluids can be a major application in horizontal, directional shale drilling applications due to formation of a barrier between
drilling mud and shale, as nano particles can easily penetrate into the shale and hence drastically reduce the shale-drilling
mud interactions and thus the shale instability problem [15].

API filter press test on samples with a fluid loss additive

The addition of fluid loss additive did not have much impact and it did marginally decrease the fluid loss from the samples,
as shown in Figure B-15. From Figure B-16 above effectiveness of the Nanoparticles as a fluid loss additive can be clearly
seen. It has better reduction in fluid loss than the standard polymer-based fluid loss additive as used in this experiment. This
may be due to the particles plugging the pores and forming an effective filter cake than the internal filter cake of the polymer.
The fluid loss values obtained with Boreplus® is lower than the samples a1, a2, a3, a4 and a5 without any additives. Thus by
using the right blends and Nanoparticles of sufficient d50 particle size concentration in the fluid, a good reduction in fluid
loss values. The mud cake formed as seen in Figure B-17 matches that formed by just polymer and surfactant blend system
indicating the wall building is internal rather than external as the Nanoparticles.

API filter press test on samples with increasing concentrations of Nanoparticles

Increasing the concentration of the Nanoparticles has a considerable effect in reducing the fluid loss of the blend mixture.
The readings from Figure B-18 confirm the same. Figure B-19 shows the comparative readings of the 90% polymer and 10%
surfactant and increasing concentrations of Nanoparticles. 10% wt/wt reading has a fluid loss of about 7.9 mL, while
increasing the concentration up to 30% has a reduced fluid loss of 5.9 mL. Thus the concentration of Nanoparticles is very
important for proper plugging of the cores in shale and also the size of Nanoparticles. As the concentration increases the fluid
loss decreases, also as the size of Nanoparticles increases the efficiency of plugging is better depending on the formation pore
sizes. 10% wt/wt is the minimum concentration required for desirable results [18].

High Temperature High Pressure filter press tests

Figure B-21 shows the results for the tests carried out in a particle plugging apparatus at 1000 psi pressure and at 200 F. The
results show clearly that surfactant is unstable at high temperatures and as a result the blend performance is not as expected as
at low temperatures.

The sample a5 consisting 50% polymer and 50% of 4% VES surfactant has a compete fluid loss as that of Sample a4 with
70% polymer and 30% surfactant performs slightly better. The fluid loss volumes are reported in standard API fluid loss,
with the original volume being doubled to compensate for the half sized ceramic disc acting as filter paper. The results cannot
be compared to the tests at room temperature in a standard filter press as the ceramic disc has 775 mD permeability and
certain porosity.

The sample with Nanoparticles performs better due to the Nanoparticles plugging the pores of the ceramic disc. However it is
not very efficient if sufficient concentration of Nanoparticles present in fluid is not in d50 particle concentration. The sample
a5 which had a complete flush was better with Nanoparticles and fluid loss was a controlled one. Fig B-23 shows a
comparison of the fluid loss at HTHP conditions for samples with and without Nanoparticles. The blends with Nanoparticles
performed better for samples with lower concentration of Surfactants. At high temperatures Surfactants are not thermally
stable and this might be the reason for high spurt loss values and also high fluid loss volumes at higher concentrations of the
Surfactants.

Care must be taken to maintain the pH of the mud at right values, if not the Nanoparticles form aggregates and gets
flocculated when subjected to pressure. The cake deposition will be irregular and not stable as shown in Figure B-27.
IPTC 14952 7

Conclusions

The Bio-Polymer – Surfactant blend is better in rheological properties and fluid loss properties than a Polymer-based fluid or
a Surfactant-based fluid. It captures the merits of both fluid systems.

The Nanoparticles play an important role in reducing the fluid loss of the individual fluid systems.

The Nanoparticles in Polymer-Surfactant blend may be used as solids free reservoir drill in fluids for drilling through shale
formations horizontally.

The Nanoparticles is effective for drilling through shale formation as it can penetrate the pores of the shale and act as a
bridging material and causing wellbore strengthening.

The amount of Surfactant plays an important role in the fluid loss characteristics. The Surfactant is not thermally stable as
Bio-Polymer at high temperatures; hence Bio-Polymer and Nanoparticles might be a good combination for high temperature
zones as Bio-Polymers are generally stable up to 350 F.

As the concentration of Nanoparticles increase the fluid loss reduces, however limited by aggregation of Nanoparticles in the
polymer fluid which may result in ineffective filter cake being developed and retard the performance of the fluid rather than
improve it.

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Acknolegments

The authors would like to acknowledge Dr. Donald Whitfill from Halliburton Co. who was instrumental in helping us to
narrow down this research and also providing the mud additives required for the experiments.

Nomenclature

API = American Petroleum Institute


bbl = Barrel
CaCO3 = Calcium Carbonate
CaCl2 = Calcium Chloride
CMC = Carboxyl Methyl Starch
cP = Centipoise
EPA = Environmental Protection Agency
°F = Degree Fahrenheit
HEC = Hydroxyl Ethyl Cellulose
HTHP = High Temperature and High Pressure
K = Consistency Index
kPa = Kilo pascals
lb/bbl = Pounds per Barrel
lbs = Pounds
nm = Nanometer
mD = Milli Darcy
IPTC 14952 9

mL = Milli liter
n = Flow Behavior Index
NP = Nanoparticles
NPX = Non-Pyruvylated Xanthan Gum
PPT = Particle Plugging Tester
PPA = Particle Plugging Apparatus
Psi = Pounds per square inch
rpm = Revolutions per minute
SBF = Surfactant-based Fluid
TTU = Texas Tech University
VES = Visco elastic Surfactant
Vol = Volume
wt = Weight

Greek Symbols
μa = Apparent Viscosity
θN = Dial Reading
μP = Plastic Viscosity
τy = Yield point
μm = micro meter

Appendix A

Table A-1: Mud weight and pH measurement

Table A-2: Mud weight and pH measurements for 20% and 30% wt/wt Nanoparticles

Appendix B
10 IPTC 14952

Figure B-1: Apparent viscosity Vs Shear rate before treatment with Nanoparticles

Figure B-2: Shear stress Vs Shear rate before treatment with Nanoparticles

Figure B-3: Apparent viscosity Vs Shear rate after treatment with Nanoparticles
IPTC 14952 11

Figure B-4: Shear stress Vs Shear rate after treatment with Nanoparticles

Figure B-5: Performance improvement after addition of Nanoparticles

Figure B-6: Rheology of Fluid Loss Additive


12 IPTC 14952

Figure B-7: Performance improvement after addition of increasing concentrations of Nanoparticles

Figure B-8: API fluid loss at 75° F for samples without addition of Nanoparticles

Figure B-9: Mud cake formation for the Surfactant-Polymer blend sample
IPTC 14952 13

Figure B-10: API fluid loss at 75°F for samples with addition of Nanoparticles

Figure B-11: comparison of API fluid loss at 75 F

Figure B-12: Mud cake formation for the Surfactant-Polymer blend sample with Nanoparticles
14 IPTC 14952

Figure B-13: Mud cake formation for the Surfactant-Polymer blend sample with Nanoparticles (after
drying)

Figure B-14: Mud cake formation for the Surfactant sample (n2) with Nanoparticles

Figure B-15: API fluid loss at 75° F for samples with FLA
IPTC 14952 15

Figure B-16: Fluid loss comparison with FLA

Figure B-17: Mud cake formation with FLA

Figure B-18: API fluid loss at 75 F for samples with higher concentrations of Nanoparticles
16 IPTC 14952

Figure B-19: Fluid loss comparison between different Nanoparticle concentrations

Figure B-20: Mud cake formation with increased concentrations of Nanoparticles

Figure B-21: HTHP fluid loss without Nanoparticles


IPTC 14952 17

Figure B-22: HTHP fluid loss with Nanoparticles

Figure 4.23: HTHP fluid loss comparison

Figure B-24: Mud cake of samples without Nanoparticles


18 IPTC 14952

Figure B-25: Mud cake of samples with Nanoparticles

Figure B-26: Mud cake of samples with Nanoparticles (after dry)


IPTC 14952 19

Figure B-27: Irregular mud cake formation due to flocculation

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