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Egyptian Journal of Petroleum (2016) xxx, xxx xxxX


Egyptian Petroleum Research Institute

Egyptian Journal of Petroleum


Enhancement of yield point at high pressure high

temperature wells by using polymer nanocomposites based
on ZnO & CaCO3 nanoparticles
a,* b c d
A.Z. Noah , M.A. El Semary , A.M. Youssef , M.A. El-Safty
Materials Department, National Research Centre, 33 El Bohouth St. (former El Tahrir st.), P.O. 12622, Dokki, Giza, Egypt

Misr Petroleum Company, Alexandria, Egypt

Packing and Packaging Materials Department, National Research Centre, Egypt

Faculty of science, Zagazig University, Cairo, Egypt

Received 6 December 2015; revised 15 February 2016; accepted 6 March 2016

po h temperature (HPHT) wells. The consequence
sit of using polymer nanocomposites based on
es different loading of ZnO-NPs and nano-
an CaCO3 on the rheological properties of oil
d base mud was evaluated and enhanced the
oil yield point at high pressure high temperature
KEYWORDS bas wells (HPHT). The using of the polymer with
e different per-centage from (0.5) in all percent
Nanocomposites; ZnO-NPs; Nano-CaCO3; HPHT; mu the obtained results is very promising; this
d means that the increase of polymer is
we reasonable for the increase of apparent
Oil base mud; Drilling fluid re viscosity, plastic viscosity and yield point at
use high temperature. Correspondingly, polymer
d nanocomposites displayed rise of apparent
for viscosity, plastic viscosity, and yield point,
dri decreased in fluid loss and increased in
llin electrical stability at high pressure high
Abstract Zinc oxide nanoparticles (ZnO-NPs) and modified calcium g temperature wells.
carbonate (nano-CaCO3) nanoparticles were successfully prepared
and added to polystyrene-butadiene rubber copolymer (PSBR) matrix h 2016 Egyptian Petroleum Research Institute.
to prepare PSBR nanocomposites. The prepared nanomaterials (ZnO- pre Production and hosting by Elsevier B.V. This is
NPs & nano-CaCO3) were characterized using scanning electron an open access article under the CC BY-NC-ND
microscope (SEM), transmission electron microscope (TEM) and X- re license (
ray diffraction (XRD). Furthermore, the prepared polymer nanocom- hig nc-nd/4.0/).X

1. Introduction
author. The inherent con-ditions standing these challenge that
E-mail address: (A.Z. of these wells cause the extreme pressures should be extremely
rheological parameters of and temperatures. considered.
Noah).X H
P fluids to differ The narrow Additionally, HPHT
enormously. Challenges boundary between wells frequently
Peer review under responsibility of Egyptian of HPHT wells include the pore pressure have high ECD
Petroleum Research Institute. the high cost essential for and fracture leading to down
the equipment and the gradient is also hole problems such
materials that are able to significant as mud losses into
1 Research Institute. under the CC
1 Production and BY-NC-ND enses/by-nc-nd/4.0/).X This is an open
hosting by Elsevier license (
3.002 access article

Please cite this article in press as:

A.Z. Noah et al., Enhancement of
yield point at high pressure high
temperature wells by using
polymer nanocomposites based on
ZnO & CaCO3 nanoparticles,
Egypt. J. Petrol. (2016),
16.03.002 X
2 A.Z. Noah et al.
mechanical properties of the (varying from 0.4 M to 0.8 M)
the formation. We, therefore, are constantly looking for new polymer com-pounds [11,12]. in methanol was added under
methods and solutions to ensure high cleaning efficiency and Moreover, ZnO is an eco- constant stirring in order to get
overcome the hazards of these over pressured formations. friendly nanoparticle and has the pH value of reactants
attracted wide attention due to between 8 and 11. These
solutions was transferred into
The cost reduction may be accomplished generally by three ways, its good antibacterialX Teflon lined sealed stainless
increasing the drilling productivity by minimizing well bore steel autoclaves and continu-
instabilities, lowering the cost of fluids and avoiding mod-ification, properties, high stability, ous at various temperature in
and over engineering of the fluid and reducing the number of photocatalytic activity and non- the range of 100200 LC for 6
platform and wells [1,2]. The configuration of dril-ling mud will toxicity [13]. ZnO-NPs have and 12 h under autogenously
depend on the requirements of the specific dril-ling operation. Holes several important applications pressure. It was then allowed to
must be drilled through different kinds of formation, requiring cool naturally to room
different types of drilling fluid. Eco-nomics, contamination, in biomedical field [14], as temperature. After the reaction
obtainable make up water, pressure and temperature are main factor food additive, and in catalysis was complete, the resulting
in drilling fluid process [3].X [15]. The incorporation of ZnO white solid products were
nanoparticles to polymers washed with methanol, filtered
matrix as nanofillers could and then dried in a laboratory
Water alone is occasionally an ideal drilling fluid and nor-mally improve not only the fabricated
used to drill areas where trouble free low pressure forma-tion oven at 60 LCX
nanocomposites, mechanical
occurs. In some areas, drilling can be started with water and the and barrier properties but also
drilled solid combined into the water resultant in a sen-sibly good create other functions and 2.2.2. Modification of CaCO3
mud. In other areas, it may be essential to add com-mercial clays to applications in food packaging nanoparticles using stearic acid
the water prior for starting drilling operation, the clay serves as dual
purpose: first, to give viscosity to the drilling fluid and second, to such as antimicrobial agent
seal the walls of the hole that the fluid circulated will not be lost to [16].X Appropriate amount of CaCO3
permeable formation being drilled. nanoparticle was added to stir-
red solution of stearic acid in
2. Experimental details
There are various mud additives that are called polymers and CH2Cl2. The mixture was
polymer nanocomposites. A strict definition of a polymer is an stirred 30 min, was then
2.1. Materials
organic chemical having a molecular weight above 200, with greater ultrasonically agitated for 30
than eight repeating units. They vary significantly in function and min, and fur-ther stirred for 24
basic properties, i.e., stability, charge. In gen-eral, polymers can be Polystyrene butadiene rubber h at 25 LC. The solvent was
copolymer (PSBR) was evaporated in vacuum and the
classified as natural, modified-natural and synthetic [4]. Many obtained from Misr petroleum residue was extracted with
types of polymer can be supplemen-tary to clear water to support in Company, Egypt. Zn
the flocculation and settling of drilled solids at the surface. When CH2Cl2 using Sox-helt
(CH3COO)22H2O (99.5%), apparatus for another 24 h until
used properly, these poly-mers used with an electrolyte for example
lime or calcium chlo-ride can keep drilling water clean and clear at zinc acetate dihydrate (99% no acid was detected in the
the suction. Polyacrylates are synthetic materials from petroleum purity) and sodium hydroxide extract. The solution was then
(pellet .99%) as the filtered and the precipitate was
feed-stocks [5]. They are not as difficult structurally as the natural introductory material were sup-
rinsed thoroughly with a
polymers and usually have a straight-chain carbon backbone with plied by SigmaAldrich
mixture of alcohol and
different side chains, depending on the desired end pro-duct. They chemicals. Calcium carbonate
deionized water. The
are usually anionic for examples: polyacrylates, copolymers, vinyl
nanoparticles (nano-CaCO3) precipitate was kept in a
acetate, vinyl polymers, and maleic anhy-dride. Their uses are: low
were supplied from Formosa vacuum oven for 24 h at 100
molecular weight (<1000)-thinners and deflocculates; medium
plastics corporation Taipei, LC. A white powder of
molecular weight (up to 100,000 MW) fluid loss control,
Taiwan and used as received. modified CaCO3 nanoparticles
flocculants and shale stabi-lizers; high molecular weight (>100,000
Cal-cium carbonate was obtained.
MW) bentonite exten-ders and flocculants. Nanocomposites based
nanoparticles with surface
on polymeric matrices gained significant importance after the report
coating of stearic acid were
of nan-oclays filled nylon-6 by [6], but the real mention of the term purchased from Malaysian 2.2.3. Preparation of
PSBR/ZnO nanocomposites
was first found in the work of [7]. Amazingly automobile tires in Nuclear Agency
which carbon black acts as a reinforcement are also an instance of a
nanocomposites. However, the term nanocom-posite is not For the preparation of
2.2. Methods
frequently used to designate such composites. Nanocomposites are PSBR/ZnO nanocomposites,
considered to be a multiphase solid mate-rial where one of the 0.5 g of polystyrene butadiene
2.2.1. Preparation of ZnO rubber copolymer (PSBR) was
phases has one, two or three dimensions of less than 100 nm
nanoparticles dissolved in 10 ml of toluene to
according to [8] and this nanocomposites used for different
obtain a 5% solution after one
applications [9,10].X In order to prepare zinc oxide hour of stirring. The
nanoparticles (ZnO-NPs) [17], PSBR/ZnO nanocomposite
In the field of materials in general and of nanocomposites in solution was set by adding
stock solutions of
particular, one of the most commonly used inorganic fillers is ZnO-NPs powder into PSB
Zn(CH3COO)22H2O (0.2 M) solution and the mixture was
calcium carbonate (CaCO3) because of its low cost, high capacity to were prepared in 50 ml
stirred for three hour and then
be dispersed in a polymeric matrix and its potential to improve the methanol under stirring. To this
sonicated for five minutes,
stock solution 50 ml of NaOH
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Enhancement of yield
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Enhancement of yield point using polymer nanocomposites

4.2 ml
Wetting agent
and the mixture is thermally aged in hot rolling with oil base mud Mud weight of this sample 1.7 ml
over for 16 h at 350 LF. After 16 h the mixture is out and the 12 PPg: Viscofire
rheological parameters are measured again using the HPHT 8g
viscometer at 120 LF (at 500 psi) and the HPHT fluid loss at 350 LF Oil=water ratio 88=12: Lime
(at 500 psi). This nanocomposite with oil base mud was used for 3g
drilling in HPHT wells. Barite
2.3. Characterization 255 g
Filter loss reducer
2.2.4. Preparation of PSBR/CaCO3 nanocomposites 2.5 g
2.3.1. X-ray diffraction (XRD) Fresh water
(33 ml water + 15 g CaCl2)
The preparation of PSBR/CaCO3 nanocomposites, 0.5 g of PSBR The crystal structure of the
was dissolved in 10 ml of toluene to obtain a 5% solu-tion after one filler powders was determined
hour of stirring. The polymer nanocomposite solution was prepared using a Philips X-ray
by adding modified nano-CaCO3 pow-der into PSBR solution and diffractometer (PW 1930
the mixture was stirred for 16 h and then sonicated for 30 min, and generator, PW 1820 resolution of 4 cm1 and 32
the mixture is thermally goniometer), equipped with Cu scans. The samples were
Ka radiation (45 kV, 40 mA, prepared by pressing 100 mg of
with k = 0.15418 nm). The KBr and 2 mg of powder to
aged in
scans of the analy-sis were run give a thin disk. A reference
in 2h range of 580L with step spectrum of a pure KBr disk is
rolling with oil base mud over
size of 0.02 and step time of 1 used.
for 16 h at
350 LF.
After 2.3.3. Scanning electron
16 h the mixture is out and the microscopy (SEM)
rheological 2.3.2. Fourier transmission
infrared spectroscopy (FT-IR) The morphology of the
parameters are measured another time using the HPHT vis-cometer nanomaterials was detected
at 120 LF and the HPHT fluid loss at 350 LF and 500 psi. This FT-IR spectra of nano-CaCO3 using a scanning electron
nanocomposite with oil base mud was used for drilling in HPHT microscopy (SEM) (High
and ZnO-NPs were achieved
wells. Resolution Quanta FEG 250-
using a Thermo Scientific
Nicolet 380 Spectrometer, SEM, Czech Republic) to
2.2.5. Preparation of oil base mud sample at Egyptian Mud USA, in the spectral range investigate the fil-ler dispersion
Engineering Company (EMEC) between 4000 cm1 and 600 cm1 and the compatibility between
polymer and fil-ler. The
with a Composition of oil base mud sample. This method involves surfaces of the samples were
in mixing of the raw materials in different percent-ages; after this, Table 1 Composition of oil base examined without coated gold
the freshwater is added to mixture drop by drop through stirrer in mud. and at low vacuum.
barrel for 1 h ( Table 1). Then they are put in thermo cup using
different temperatures. The next step is to measure the mud rheology Diesel 2.3.4. Transmission electron
by HPHT viscometer. Controlling mud weight depends on the microscopy (TEM)
238 ml
percentage of diesel and barite.X Emulsifier
The structure and surface morphology of the prepared ZnO-NPs and of emulsion stability is The XRD patterns of ZnO
its nanocomposites were studied using JEOL JEM-1230 generally smooth, shiny and nanoparticles and PSB/ZnO
transmission electron microscope (TEM) with accel-eration voltage does not adhere to the stirring nanocomposites are displayed
of about 80 kV. The nanocomposite samples were prepared by spindle of a mixer. By con- in Fig. 1. The XRD profile
adding a small drop of the dispersion of polymer bio- trast, a mud with a low degree ZnO-NPs showed characteristic
nanocomposites onto a Lacey carbon film-coated copper grid and of emulsion stability is dull, peaks corresponding to the
allowed to dry initially in air then by applying high vacuum grainy and shows a marked planes (100) at 2h = 30.74L,
tendency adhere to the spindle. (002) at 2h = 34.5L, (101) at 2h
The oil wetness or oil wetting = 36.8L, (102) at 2h = 47.7L,
tendency of an invert emulsion (110) at 2h = 56.2L, (103) at 2h
3. Results and discussion mud is defined here as the = 61.7L and (112) at 2h =
ability of the mud to 67.6L. This XRD pattern shows
In this paper, the authors offer a solution to one of the most incorporate foreign materials that the preparation of ZnO-
significant challenges of the drilling fluids in HPHT (high pres-sure into the external, or oil phase. NPs leads to wurtzite phase and
high temperature) wells circulation as ( Table 2); carrying the drill A mud with high emulsion all the diffraction peaks agree
cuttings back to the surface for continuous polymers has been stability is phase. A mud with with the reported JCPDS data.
widely used as drilling additives because of their unique structure high emulsion sta-bility is oil This was confirmed by TEM
that makes them able to plug pores, and stand the high temperature wet, by definition, but may not observation, in which ZnO-NPs
and pressure conditions. Conversely, the properties of the mud can necessarily be oil wetting. appear as spherical particles
be further enhanced by using nano-materials that can enable the with size around 6 nm as shown
drilling fluid to function better under extreme conditions. X in ( Fig. 2). Furthermore, the
3.1. Structure of ZnO XRD patterns ofX
Electrical stability (ES) of an oil base mud is considered a measure nanoparticles
of its emulsion stability. In the laboratory, a mud with a high degree
Please cite this article in high temperature wells by using polymer nanocomposites
press as: A.Z. Noah et al., based on ZnO & CaCO3 nanoparticles, Egypt. J. Petrol.
Enhancement of yield
point at high pressure X
4 A.Z. Noah et al.

Table 2 Influence of polymer nanocomposites based on modified nano-CaCO 3 and ZnO-NPs on oil base mud.

Before hot rolling
After hot rolling
Before hot rolling/after point
pressure 500 psi)

(temperature 120 LF, pressure

(temperature 300 LF, pressure
RPM Results PV Yield
Fluid loss (ml/30 min)
RPM Results PV Yield Before hot
E. stability
(beek volt)
500 psi)
500 psi)
e 300 LF,
(temperature 120 LF,
500 psi

29 0.5 ZnO-NPs
Blank (PSBR) 6
600 10
200 26
28 600
600 6
58 9
with 0.5 PSBR
after 300
16 h 57
300 100
38 22
8 300
300 100
36 22

after 16 h
200 6
0.5 modified
29 10
77 200
27 40
200 6
28 9
nano-CaCO3 100
300 34
100 3
22 8
300 33
100 3
22 8

with 0.5 g. PSBR

200 6

6 12


indinsmission electron microscopy Fig. 3) ZnO corresponds to

cat (TEM) nanoparti-cles that of pri-
es (average size, mary particles,
that Single crystalline ZnO 6 nm) are except for a
Zn nanoparticles were manufactured found to be very few
O- by a hydrothermal method; zinc homogeneousl agglomerates.
NP acetate and 0.5 M NaOH were y dis-persed in X
s used to prepare ZnO-NPs at 150 the PSBR
fill LC for 6 h using absolute ethanol. matrix. The
ed TEM image confirms the efficiency of 3.1.3. Infrared
em formation of ZnO-NPs with an nanoparticles (IR) spectral
Figure 1 XRD pattern of bed average size around 6 nm, which in improving analysis
ZnO-NPs as well as
intois in good agreement with XRD the properties
pol of the polymer In order to
ym results ( Fig. 2). The ZnO-NPs in material is establish
er the range of nanometer grade primarily probable
mat have a good dispersibility in determined by intermolecular
rix PSBR matrix. The dark zones the degree of interactions
con correspond to the crystalline dispersion in among
- ZnO-NPs although the bright the matrix. components in
sist zones point to the amorphous These the system,
exhibited a broad,
s of PSBR matrix, because of the high nanostructured FT-IR
noncrystalline peak of
two electron density of the ZnO- ZnO in the spectroscopy
polymer and more
- NPs.X polymer can mea-
intense and crystalline
pha change the surements
diffraction peaks of
se 3.1.2. Scanning electron thermal and were carried
ZnO-NPs. The
stru microscopy (SEM) optical out. Fig. 4
occurrence of ZnO-
ctur properties of FT-IR spectra
NPs creates
es. the composite. of ZnO-NPs,
SEM images were obtained using The size of the
a voltage of 20 kV. The sur-faces the bands
3.1. of the ZnO-NPs and PSBR/ZnO ZnO observed at
neither new peak nor 1. nanocomposite films were nanoparticles 424, 453, and
peak shifts with Tra in the PSBR
studied using SEM are shown in ( matrix 527 cm1 areX
respect to PSB which
et hancement of yield point at high based on ZnO Egypt. J.
al., pressure high temperature wells by & CaCO3 Petrol. (2016), rg/10.1016/j.ejpe.2016.03.002 X
Please cite this article En using polymer nanocomposites http://dx.doi.o
in press as: A.Z. Noah nanoparticles,

Enhancement of yield point using polymer nanocomposites

Figure 2 (A and B) TEM of ZnO-NPs prepared by hydrothermal method and PSBR/ZnO nanocomposite.

Figure 3 SEM images of (A) ZnO-NPs, (B) PSBR/ZnO nanocomposite.

[18,19] out of which the bands
at 453 and 527 cm1 are present
in the ZnO-NPs spectrum con-
firming the formation of ZnO-
NPs. The three bands centered
at 1338, 1412, and 1572 cm1
detected in the ZnO-NPs spec-
Figure 4 FT-IR spectra of ZnO- trum are ascribed to the
NPs. stretching vibrations of CO,
CC, and CAH groups in acetate
species. The favorableX

assigned to Zn-O vibrations intermolecular interactions

between these groups and nanoparticles affected the variations in the crystalline and nanoform which using TEM and SEM. Fig. 6X
characteristic absorption bands. revealed that the calcium
carbonate is described by two
characteristic crystal phases: (b) exhibited the TEM images
3.2. The surface morphology of modified CaCO3 nanoparticles of modified CaCO3 nanoparti-
aragonite and calcite.X
cles using stearic acid. Also,
3.2.1. X-ray diffraction patterns (XRD) Fig. 6(a) represented the SEM
3.2.2. Transmission electron
microscopy (TEM) and SEM image of modified CaCO3
Fig. 5 displays the analysis of crystal structure using XRD for nanoparticles using stearic acid.
nano-CaCO3 powders. The results established that the chief The morphology structure and It is shown in Fig. 6(a) that
diffraction peaks of the crystalline structures of the nano-CaCO 3 are the dispersion of CaCO3 some of the modified CaCO3X
in the range 25L55L. This indicates the presence of nano-CaCO3 in nanoparticles were carried out
Please cite this article in high temperature wells by using polymer nanocomposites
press as: A.Z. Noah et al., based on ZnO & CaCO3 nanoparticles, Egypt. J. Petrol.
Enhancement of yield
point at high pressure X
6 A.Z. Noah et al.
confirmed that the phenomena
of nanoparticles agglomeration
decreased effectively because
the nanoparticles were kept
apart by the surface-
modification layer of stearic
acid and increased the activity
of the modified CaCO3
nanoparticles. A few studied Figure 7 FT-IR spectrum of the
the surface modification of CaCO3 nanoparticles.
CaCO3 nanoparticles by stearic
acid and the effect ofX modified-CaCO3 nanoparticles
cannot be stably dispersed in
non-polar organic solvents.

3.2.3. Infrared (IR) spectral


From the FTIR spectrum of

CaCO3 nanoparticles illustrated
in Fig. 7, it can be seen that
Figure 5 The XRD patterns of nano-CaCO3 powder.
the CaCO3 nanoparticles had
adsorption bands at 29502840
cm1, corresponding to the
nanoparticles were seriously aggregated and lapped over and the vibration mode of CAH of
particle size ranged from 64 to 100 nm. Also, it was shown from stearic acid, and also 707,
Fig. 6(b) that stearic acid modified nano-CaCO3 was dis-persed well 873X
and individual nanoparticles could be distin-guished. These results


Figure 6 SEM image of modified nano-

CaCO3 (a) as well as TEM image (b)
with different magnifications.

article in press as: pressure high temperature wells by

A.Z. Noah et al., using polymer nanocomposites based Egypt. J. Petrol. (2016),
Enhancement of
on ZnO & CaCO3 nanoparticles,
Please cite this yield point at high X
Enhancement of yield point using polymer nanocomposites

In general, high gel strength of the increase of apparent

1 mud increases the viscosity. viscosity, plastic viscosity and
and 1418 cm corresponding to the in-, out-plane bending and
Nonetheless, this is not always yield point at high tem-
asymmetrical stretching vibration peaks of OACAO, respectively. true because the high viscosity perature. Consistently, the
They all are characteristic peaks in calcite [20,21].X can be accomplished when the prepared nanocomposites
dispersion of clays in the mud demon-strated increase of
3.3. Influence of PSBR nanocomposites on properties of mud is apparent viscosity, plastic
rheology viscosity, and yield point,
excessive. From this study, decrease in fluid loss and
adding zinc oxide nanoparticles increase in electrical stabil-ity
From Table 2 when adding 0.5 of modified calcium carbonate with at high pressure high
and modified calcium
0.5 of the PSBR polymer on oil base mud, it was observed that the carbonate nanoparticles to the temperature wells. From all the
yield point increased from 16 to 23, and the fluid losses decreased oil base mud will influence obtained results, ZnO-NPs and
from 12 to 7 while the electrical stability increased from 850 to yield point, gel strengths, fluid modified nano-CaCO3 as well
1550. Also, the addition 0.5 of ZnO-NPs to 0.5 PSBR polymers, losses and electrical stability, as polymer nanocomposites are
significant increases are observed in both the plastic viscosity from and these unique nanoparticles novel materials that can be used
22 to 31 and yield point from 16 to 26, whereas the fluid losses can be uti-lized as fluid for high pressure high
decreased from 12 to 6 and the elec-trical stability increased from viscosity stabilizer to temperature wells (HPHT)
850 to 1850 beek volt. From this result we can conclude that the significantly improve the owing to the improvement of
using of polymer nanocompos-ites based on ZnO-NPs enhanced the cutting recovery. yield point, increasing electrical
yield point at high pres-sure high temperature wells more than stability and declining fluid
polymer nanocomposites based on modified nano-CaCO3.X losses.
4. Conclusion
3.4. Effect of viscosity (yield point) on cutting recovery, fluid losses
and electrical stability on mud rheology References
The present work has revealed
that the preparation of ZnO-
The viscosity of oil base mud increases as the amount of poly-mer NPs by a hydrothermal method
N. Danvers, Fluid Mechanics,
nanocomposites containing zinc oxide nanoparticles and modified and modification of nano-
calcium carbonate nanocomposites increase. Table 2 shows the Addison-Wesley Publishing
CaCO3 then using the prepared
effect of adding polymer nanocomposites loading with ZnO-NPs Company, 1977. X
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and modified nano-CaCO3 to oil base mud exciting capacity for polymer(PSBR)
various flow rates. The percentage of the cutting recovery displays nanocomposites based on nano- Standard Procedure for Testing
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Fluid losses decreased as the nanocomposites containing ZnO-NPs successfully fabricated by a Drilling Fluids, API RP 13B-1,
second ed. , American Petroleum
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depend on the cutting size and annular velocity. The enhance-ment polymer nanocom-posites were X
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compared to the bigger cutting size. Moreover, the improvement in IR and TEM. The SEM
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Composition and Properties of Oil
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press as: A.Z. Noah et al., based on ZnO & CaCO3 nanoparticles, Egypt. J. Petrol.
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point at high pressure X

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Please cite this article in press as: A.Z. Noah et al., Enhancement of yield point at high
pressure high temperature wells by using polymer nanocomposites based on ZnO &
CaCO3 nanoparticles, Egypt. J. Petrol. (2016), X