SPE-174260-MS

Mitigation of Formation Damage and Wellbore Instability in Unconventional

Reservoirs Using Improved Particle Size Analysis and Design of Drilling
Fluids
J. Dorman, Independent Consultant, Szolnok; I. J. Lakatos, Res. Inst. Applied Earth Sciences, UM, and MOL
Plc., E&P Division, Miskolc/Budapest; G. Szentes, Res. Inst. Applied Earth Sciences, UM, Miskolc; A. Meidl,
HOST Ltd., Budapest, Hungary

Copyright 2015, Society of Petroleum Engineers

This paper was prepared for presentation at the SPE European Formation Damage Conference and Exhibition held in Budapest, Hungary, 35 June 2015.
This paper was selected for presentation by an SPE program committee following review of information contained in an abstract submitted by the author(s). Contents
of the paper have not been reviewed by the Society of Petroleum Engineers and are subject to correction by the author(s). The material does not necessarily reflect
any position of the Society of Petroleum Engineers, its officers, or members. Electronic reproduction, distribution, or storage of any part of this paper without the written
consent of the Society of Petroleum Engineers is prohibited. Permission to reproduce in print is restricted to an abstract of not more than 300 words; illustrations may
not be copied. The abstract must contain conspicuous acknowledgment of SPE copyright.

Abstract
The key to formation damage control is minimizing the depth of contact/impact of the formation and
drilling fluid by minimizing solids and liquid invasion into porous (fractured) formations. Analysis of
downhole filtration conditions and particle size (distribution) measurements were used to select fit to
pore size fluid loss control materials in order to maximize pore/fracture plugging efficiency. Further tests
served to predict potential alteration of rock properties. Particle size measurements have been performed
for commonly used (natural and synthetic) polymeric fluid loss and other additives dispersed in water.
High-pressure Hg porosimetry was used to determine the pore size distribution of core samples. Core flow
tests served to measure permeability and permeability damage caused by fluid loss additives. Spontaneous
fluid absorption rate was studied using modified tensiometer and wettability of the cores were determined
by sitting drop technique.
In low permeability porous (tight and shale gas) formations consisting of macro to nano pores most
filtration studies are limited to provide reliable filtration data for all cases due to the fact that drilling fluids
solids particle sizes relative to pore sizes. Particle size measurements of commonly used (natural and
synthetic) polymeric fluid loss additives in water have provided typical size range by particle number in
the 25-35 nm range, and 120-700 nm by volume. Such particles can play a significant role in internal
plugging of micro to nano size pores and microfractures. Core flow/filtration tests using low permeability
(5 mD) core samples and model fluids containing fluid loss additives resulted in rapid permeability
reduction (to 100%), typically in close to core face region. Results proved the achievable pore plugging
efficiency and invasion control into low permeability rocks during drilling. Particle size data gained for
CPG (Cloud Point Glycol) solutions proved that this system could also be used to form efficient barrier
within the low permeability formation, showing certain analogy between mitigation of formation damage
and wellbore instability. Better insight into downhole filtration mechanism and conditions, especially for
initial filtration phase in low permeability formations can lead to designed shallow bed instead of
practically uncontrolled deep bed filtration, where external filter cake is essentially not formed. Such

SPE-174260-MS

internal pore plugging technique can be the key to the minimization of solids/liquid invasion and
associated formation damage.

Introduction
Formation damage potentials and associated risks in unconventional (i.e. tight gas, shale gas) formations
during drilling (and other well operations) and finding solutions have long been studied (Bennion et al.,
1996). The interest in this topic still exists and numerous technical and scientific papers provide
significant contribution to better knowledge and understanding of the very complex area. These formations are extremely prone to formation damaging effects (McPhee et al., 2008). The difficulties mainly
come from typically low pore sizes (10 - 1000 nm) and in many cases from rock mineralogy (Akanji et
al., 2013). Detailed study of formation rocks properties (Riepe et al., 2011) is essential to fit- to-purpose
drilling fluids design (Franks et al., 2011). Studies on reservoir engineering (Clarkson et al., 2011) and
correlation of core data and logging results (Ramakrishna et al., 2010) further improves the knowledge in
fighting against formation damage. Research and design of new drilling fluids based on complex
assumptions have led to more and more sophisticated fluid formulations including the use of nanoparticles (Zakaria, 2013). Almost in all studies, the filtration of drilling fluids is thought to be the main
source of formation damage (Dabiri, 2013). Filtration tests performed either under static or dynamic
conditions (Jin, 2009) are considered one of the best approaches in formation damage control.
The practical approach to minimize filtration rate and solids/liquid invasion is based on enhanced pore
plugging efficiency achieved by optimization of bridging agents particle size distribution (Abrams, 1977
and Vickers et al., 2006). However, the size ranges of solid drilling fluid additives, bridging and weighting
agents, drilled solids are typically in the m to mm range that is far from nano ranges of the pore sizes.
This fact enforces to revise the applicability of classic theories of filtration and pore blocking in relation
to low permeability formations. On the other hand, the invasion of drilling fluids filtrate into the porous
formations increases the pore pressure and that can lead to loss of near-wellbore true overbalance pressure,
which can cause wellbore instability. Drilling fluid additives, which can minimize the rate of fluid
invasion, help to maintain wellbore stability (Ewy et al., 2008).
Other factors in addition to near wellbore pore pressure increase caused by filtrate invasion are the
redistribution of rock stress conditions and softening (weakening) of the rocks in case of water-based
drilling fluids (Pagels, 2014). Both factors reduce the mechanical strength of formation and increase the
tendency of borehole destabilization. Most of the conventional filtration control additives cannot prevent
filtrate invasion and pressure penetration because of small (nano-range) pore sizes and the fact that
external filter cake does not form on the formation face. Fortunately new techniques (i.e. the use of
nanomaterials) for filtration (fluid invasion) and formation damage control meet with the efforts made for
the mitigation of wellbore instability as well (Relay et al., 2012).

Background
Internal/external filter cake buildup during drilling fluids filtration
During overbalanced drilling through the porous formations the drilling fluid tends/is forced to penetrate
into the pore matrix. In the initial phase of drilling fluids downhole filtration - known as spurt loss - the
liquid phase and small size solid particles (smaller than pore throats) invade the near wellbore region.
Invading solid particles are trapped within the porous matrix and in association with high molecular size
solubilized/dispersed components of drilling fluid (i.e. fluid loss control additives) start to form a reduced
permeability zone of internal filter cake. The larger size (relative to pore size) solid particles are retained
by extrusion and clogging on the porous rock surface and in association with smaller solid particles and
high molecular size solubilized/dispersed components of the drilling fluid tend to buildup the external
filter cake. The ultimate task of drilling fluids technology and engineering is to build up the possible
lowest permeability and thin filter cake, preferentially on the formation face at minimum solids/liquid

SPE-174260-MS

invasion into the formation. Downhole filtration behavior of drilling fluids is approached/modeled by
laboratory filtration tests. Test results of standard or special (i.e. HTHP - high temperature and high
pressure) filtration measurements (using filter papers) provide mainly comparative results and rough
estimation of related wellbore processes and refer to external filter cake properties only. Modified
laboratory methods using synthetic filter media (porous ceramic or aloxite discs, and cylindrical core) or
synthetic and natural core plugs give more reliable, more realistic results involving effective pore plugging
ability of drilling fluids solids components.
HTHP filtration tests (107 C and 2.1 MPa differential pressure) using ceramic disks (10 m pore size)
gave a good general figure of static filtration process in contact with porous media (Elkatatny et al., 2012).
Filter cakes formed during static/dynamic tests consisted of two layers of different thickness and physical
properties as shown by 2D CT scan. A thinner bottom layer and thicker top layer were observed after
filtration (both layers were thinner under dynamic conditions). The external filter cake had low (0.087 d)
permeability. The relatively high spurt losses and substantial reduction (by 35-40 %) of ceramic disks
porosity indicated high solids invasion and poor bridging. Poor pore bridging and deeper solids/liquid
invasion can be the result if the particle size distribution (PSD) of bridging agent is not properly fitted to
actual pore size distribution. According to the one-third (Abrams, 1977) theory optimum pore plugging
can be achieved if the mean particle size of the bridging agent is equal to one- third of mean pore size.
Including this criterion by Vickers et al. (2006) has fine-tuned the design procedure considering a better
fit of particle and pore size distributions. Successfully used software are now available in the industry for
this purpose, highlighting the role and importance of bridging agents PSD in drilling fluids filtration
optimization and minimization of formation damage. Results of other studies (Longeron, 2000, Jin, 2009)
dealt with dynamic mud filtration under simulated downhole conditions clearly differentiate between
initial rapid filtration (spurt loss) and stabilized section of dynamic fluid loss (see Fig. 1).

Figure 1Filtration behavior of drilling fluids under simulated wellbore conditions (after Longeron, 2000)

SPE-174260-MS

In general, these sections refer to internal and external filter cake buildup respectively. The actual,
dynamic bottomhole conditions and the consideration of their potential effects are critical in the estimation
of downhole filtration and invasion characteristics when drilling new wellbore sections.
Bottomhole shear conditions affecting filter cake buildup
In laboratory dynamic filtration studies the typical annular shear rate ranges within the operating win dows
are used to simulate shear forces generated by drilling fluid flow at the wall of wellbore (Jin, 2009), which
may strongly influence the internal/external filter cake deposition and fluid loss/invasion control. The
initial phase of real downhole filtration (deposition of internal and external filter cake) is primarily
governed by the special bottomhole flow conditions determined by typical bit geometry and hydraulics.
Typical drilling fluid flow profile at and around the bit was shown by Deen et al. (2014) using
computational fluid dynamics analysis. The impinging fluid jet flow, upward directed flow path, spiral
orientation created by bit geometry and bit rotation, reduced flow area caused by bit geometry generate
unique flow conditions in the bottom hole section. The effect of high drilling fluid velocity along the new
drilled circumferential segments of the wellbore wall (at each bit rotation) provides unexpectedly eroding
flow conditions to internal/external filter cake deposition on the virgin rock surface even for tens of
minutes depending on actual drilling rate. Therefore the control of internal filter cake deposition and its
properties come to priority if the deposition of external filter cake is unlikely under bottomhole conditions
in case of low permeability (low pore size) formations due to solids particle size to pore size ratio.
Potential factors in downhole filtration into low permeability formations
The unconventional reservoirs (e.g. tight sands, gas shales) are typically low permeability formations. The
neighboring formations to be drilled through prior to encountering potential pay zones can widely vary
from very low permeability shales (including cap rock) to compacted permeable sands. Actual downhole
drilling fluid filtration into each of these different formations is the key factor to fulfill successfully the
technological requirements.
At each bit rotation downhole filtration into the formation through the virgin rock surface starts by
dynamic filtration and internal filtercake buildup. The drilling fluid stream directed upward from the
bottom flows essentially parallel to the wall of the wellbore at difficult to define flow path of high velocity
(much higher than in the stabilized annular flow at drillpipe). Fig. 2 illustrates the forces acting on a solid
particle, which tends to deposit on the surface of the filter cake (Farajzadeh, 2004).

Figure 2Forces acting on a particle deposited on the surface of the filter cake (after Farajzadeh, 2004)

SPE-174260-MS

The same forces act on solid particles (bentonite, barite, bridging agent, drilled cuttings, etc.) carried
by the fluid flow close to the wall of the wellbore. In the bit zone, the extremely high shear/drag forces
carry the larger and smaller particles upward and prevent the smaller ones from entering into the porous
matrix and blocking the pore throats. Very likely the particles smaller than pore size (typically 100 nm)
can enter, deposit and block (by adhesion or clogging) the small size pores. The classic theory of pore
plugging (considering the common particle size distribution of drilling fluids) cannot be used in this case.
Therefore, the liquid phase of the drilling fluid (and its components) can play primary role in filtration/
invasion control rather than the solid phase. Small (nano) size components of drilling fluids liquid phase
can effectively block small size pore throats by strong adhesion to the pore wall and attractive interparticle
forces due to very high surface area and/or molecular interaction. Because of wide range of low
permeabilities and pore sizes (from micro to nano) according to classic bridging theory (Abrams, 1977 and
Vickers et al., 2006) a wide range of nano (and micro) sized particles in proper concentration should be
available in the drilling fluid for best bridging/plugging performance. The question is to what extent does
the present field practice meet with this criterion under real drilling conditions? Lack of internal filter cake
lead to deeper invasion and associated high velocity fluid stream transports fine solid particles deeply into
the formation (deep bed filtration) or can cause induced fines migration. It should also be considered that
high overbalance pressure could lead to detrimental effect in case of lack of internal filtercake. High
temperature is another important factor to be considered in Hungary from both formation damage and
wellbore instability point of view. Filtration rate is strongly influenced by elevated temperature based on
complex physical and colloid-chemical factors.
An integrated engineering approach: analogy between control of formation damage and wellbore
instability
It is widely analyzed and usually concluded that invasion of solids and liquid of drilling fluids into
porous/permeable formations during drilling leads to formation damage, which normally means variable
depth of invasion and associated permeability reduction (permeability damage). This topic has been
thoroughly studied by numerous authors and is still an ever-actual theme of new research/development
works in relation to achieve better insight into potential factors and mechanism, development of new
nondamaging drilling/completion fluids and techniques in order to minimize formation damage when
drilling through producing formations (pay zones). The major focus in these studies is to minimize solids
and liquid invasion, formation rocks and drilling fluid interactions through effective filtration control, and
to achieve easy to restore downhole/formation conditions to maximize productivity if necessary.
On the other hand fluid invasion especially into low permeability (i.e. tight sand and/or shale)
formations normally causes wellbore instability due to invading filtrate generated pressure penetration and
rock/shale fluid interactions (i.e. hydration and weakening). Potential of pore pressure penetration in the
near wellbore area and efficiency of additives can be evaluated using PPT (pore pressure transmission)
tests (Stowe et al., 2001). Such wellbore instability problems may be further enhanced in presence of
drilling induced microfractures. One of the most efficient solutions for mitigating wellbore instability is
to minimize fluid invasion by effective plugging of typically small size pores and forming of physical
barrier in the near wellbore region. Temperature clouding polyglycols and alcohol-alkoxylates (TAME)
have been successfully used from the early 90s for shale stabilization in water-based muds (WBM)
essentially by pore and microfracture plugging (van Oort, 2003). Specially formulated micronised
deformable sealing polymer (MDSP) was also used to seal microfractures and to control wellbore
instability while drilling through interbedded shale and tight sand (Vickersburg) formations (Hoover et al.,
2008). Sulfonated asphalt based products are also field proven additives. Nanoparticle- containing drilling
fluids were developed for hydrocarbon bearing shale (gas) formations to minimize wellbore instability and
formation damage (Sharma et al., 2014). While nanopores of shales are sized typically in the 5-50 nm
range, mezo- and micropores and microfractures (induced or natural) represent additional wide size range

SPE-174260-MS

of openings to be plugged/sealed in low permeability (i.e. unconventional) formations in the drilling

practice. Therefore, a wide range of particle sizes and proper size distribution of filtration control additives
are required to minimize fluid invasion. Consequently, very similar drilling fluids engineering approach
can be applied for efficient control of formation damage and wellbore instability.

Laboratory experiments and discussion of results

Filtration control, or in other words, fluid loss additives are primarily tested/evaluated for their efficiency/
performance in filtration tests focusing on external filter cake buildup and filtration rate (cake permeability) reduction. However, these tests are limited to provide reliable data for their potential pore plugging
efficiency in low permeability formations, where external filter cake formation is delayed. As it was
discussed in the previous section, these additives can also play positive role in downhole dynamic
filtration by reducing the permeability in the near wellbore region and controlling fluid invasion.
Particle size measurements of fluid loss control additives
Based on previously detailed approaches we have performed laboratory test to determine the particle sizes
of selected three polymeric fluid loss control additives (and high temperature stabilizers) that were
successfully used in several high temperature drilling applications in Hungary (Dorman, 2010). The
drilling fluid additives used for laboratory tests were selected from the group of sulfonated, temperature
stable and salt tolerant polymers specifically developed for HTHP drilling fluids: P1 (synthetic sulphonated polymer of low molecular weight), P2 (synthetic sulphonated polymer of medium molecular
weight), V3 (sulphonated natural-based polymer derivative). The objective of the laboratory tests was to
study the structure and disperse character of the additives and to determine the disperse phase, drop and
solid particle sizes and size distributions in water solutions at various concentrations.
The tests were performed using low-angle Back Scattering Laser Photon Correlation Analyzer and
Nanosizer at 25 C. In these tests, intensity, volume and number of particles determined the sizes and size
distributions of dispersed particles. From the large number of tests results only the particle sizes by
volume data were illustrated representatively. The designed fluid loss additives may contribute to internal
filter cake buildup by pore blocking and permeability reduction in low permeability formations by
volumetric pore plugging therefore particle size distribution data by volume were primarily analyzed.
The particle size distribution by volume curves in Fig. 3 shows that in 1 g/l solution of P1 the small
size (50-90 nm) and large size (250-450 nm) particles represent 70% and 30% of the particles respectively.
These two data can be used for characterizing the structure of the polymer solution. The particle size
analysis of the 50 g/l solution (Fig. 4) represents an extreme case (in concentration) at the same time it
can provide better insight into the structure of the system and molecular interactions. Data prove that with
increasing of concentration of P1 polymer the tendency for aggregation is increasing. The size distribution
tests results for the solutions of P2 (Fig. 5 and 6) are similar to the distribution curves for the same
concentration of P1 solution.

SPE-174260-MS

Figure 3Size distribution by volume of 1 g/l P1 solution

Figure 4 Size distribution by volume of 50 g/l P1 solution

Figure 5Size distribution by volume of 1 g/l P2 solution

SPE-174260-MS

Figure 6 Size distribution by volume for 50 g/l P2 solution

It can be concluded that, although the molecular weight of the two products may differ, the sizes of
the aggregates are close to each other and with increasing of concentration; the tendency for aggregation
of P2 is also significant. It is interesting however, that in spite of higher molecular weight, the aggregation
tendency of P2 polymer is lower compared to P1. Considering the aggregation tendency of the products,
the gel domains, the microgel formed because of intermolecular interaction can be attributed to the
700-800 nm peaks, while the particles larger than 1000 nm (1 m) consist of insoluble, visible and
relatively quickly settling components.
The data gained for the 50 g/l solution of V3 show a different picture as compared to the results of the
other two samples. The particle size average of V3 is the greatest of all three products. The particle size
distribution by volume curves in Fig. 7 show that in 1 g/l solution of V3 the small size (150-300 nm) and
large size (650-850 nm) particles represent 80% and 20% of the particles respectively. The particle size
analysis of the 50 g/l solution of V3 (Fig. 8) also proves that with increasing of concentration of polymer
the tendency for aggregation is increasing. The size distribution test result for the solution of V3 (Fig. 8)
shows a significant change in particle sizes by volume and the ratio of small and large size particles has
changed to 35% and 65% respectively. It is worth mentioning, however, that large aggregates (1000 nm)
have not been formed compared to P1.

Figure 7Size distribution by volume for 1 g/l V3 solution

SPE-174260-MS

Figure 8 Size distribution by volume for 50 g/l V3 solution

The concentration dependence of the particle sizes shown in Fig. 58 refers to the fact that based on
the macromolecular character of P1 and P2 the size increase can be attributed to intermolecular
interaction. The behavior of P1 and P2 is similar, with the increasing concentration the average particle
size of the disperse part increases due to the formation of aggregates (gel domains). The behavior of V3
additive differs from the others as the increase of average particle size is much less with increasing
concentration. This is probably the consequence of the fact that this natural material forms monomolecular
solution, the dissolved material has relatively low tendency to aggregate. However, behind the above
general conclusions a significantly more complex picture emerges with regard to structure and dispersity
of solution, if the particle size distribution is evaluated on the basis of intensity, volume and number. The
comparison shows that the number of the small particles is prevailing (the distribution curve by number
is mono-modal), although the dispersed phase of the solution contains substantial amount of larger size
disperse components (the distribution curve by volume is multi-modal).
Selection and characterization of core samples-I
Low permeability core samples were selected for filtration tests using laboratory prepared solutions of the
fluid loss additives characterized in the previous section to simulate the filtrate invasion and associated
permeability reduction within the core matrix before external filter cake can start to form. It is assumed
that this is typically the case at least for several minutes at the bit region during drilling of new sections
in low permeability (i.e. unconventional) formations.
The data of the core plugs used for the filtration test at 30 C are shown in Table 1 Table 3, while
pore size distribution data can be seen Fig. 911. What the absolute and the differential pore size
distribution curves had in common was that although the average pore size was ~4,5 m, the micro
porosity of the cores and the number and volume of the 10-1000 nm pores are significant.

Table 1Mercury injection data obtained from core plug A

Total injected volume:
TOTAL specific surface:
Average pore radius (Micron):
Porosity:
Density:
Matrix density:
Macro porosity (up to 2 bar)
Micro Dorositv (above 2 bar)

0.0935
1.1830
4.5685
20.21
2.1607
2.7080
8.47
11.74

cm3/g
m2/g
m
(%)
g/cm3
g/cm3
(%)
(%)

10

SPE-174260-MS

Table 2Mercury injection data obtained from core plug B

Total injected volume:
TOTAL specific surface:
Average pore radius (Micron):
Porosity:
Density:
Matrix density:
Macro porosity (up to 2 bar)
Micro porositv (above 2 bar)

0.1304
1.4640
4.2765
20.51
1.5732
1.9792
7.52
12.99

cm3/g
m2/g
m
(%)
g/cm3
g/cm3
(%)
(%)

Table 3Mercury injection data obtained from core plug C

Total injected volume:
TOTAL specific surface:
Average pore radius (Micron):
Porosity:
Density:
Matrix density:
Macro porosity (up to 2 bar)
Micro porosity (above 2 bar)

0.0929
0.9640
4.5745
19.93
2.1455
2.6796
8.23
11.71

Figure 9 Pore size distribution of core plug A

Figure 10 Pore size distribution of core plug B

cm3/g
m2/g
m
(%)
g/cm3
g/cm3
(%)
(%)

SPE-174260-MS

11

Figure 11Pore size distribution of core plug C

Core flow test results, filtration study-I

The objectives of the laboratory filtration tests were to determine how the injection of synthetic formation
water containing the additives in 10 g/l concentration influences the permeability of the natural cores pore
system and what kind of return permeability characterizes the reverse injection of water. In lowpermeability core plugs cut from the same zone the following injection protocol has been performed:
1. Saturation of the core with formation water,
2. Determination of the balanced permeability for water (injecting 100 ml formation water),
3. Injection of formation water based solutions containing the additives in 10 g/l concentrations and
measuring the permeability continuously,
4. Reverse injection of water,
5. Recording the water permeability continuously and determining the return permeability after the
injection of 100 ml formation water and calculating the changes (% of permeability damage).
The mobility values, calculated based on the measured data in relation to the volume of the injected
fluid can be seen in Fig. 12 14.

Figure 12Filtration test of P1 solution (10 g/l) using core plug A

12

SPE-174260-MS

Figure 13Filtration test of P2 solution (10 g/l) using core plug B

Figure 14 Filtration test of V3 solution (10 g/l) using core plug C

Evaluation of the core flow tests data (Fig. 12 14) showed that the permeability of cores during the
injection of synthetic formation water gradually decreased but at different rate although the core plugs
were cut from the same block. At the end of injection of 100 ml formation water the permeability vs. water
was 17.77 mD, 12.65 mD and 9.35 mD for Core A, B and C respectively. The permeability was calculated
from the mobility data assuming 10 mPas dynamic viscosity. According to the test program 100-100
ml of the three solutions containing 10 g/l additives would have been injected, this intention could only
be realized for the solution of P1. 50 ml of P2 solution, while only 30 ml of V3 solution could be injected
because of dramatic permeability decrease. According to the test data (Fig. 12), core A maintained the
high permeability after water injection and this can be attributed to the fact that the planned 100 ml of P1
solution could be injected. The mobility was 1.397 mD/cP, which multiplied by the viscosity ( 1.269
mPas) of the solution results in 1.772 mD permeability. Following the above approach it can be stated that
after the injection of 50 ml of P2 solution the mobility decreased from the initial 12.65 mD/cP to 0.0345
mD/cP, which considering the 1.636 mPas viscosity of the solution corresponds to 0.0564 mD, i.e. 56.4
D. In the case of injection of 30 ml of V3 solution, the mobility rapidly decreased below 0.01 mD/cP
and stabilized at 0.006 mD/cP. Since the viscosity (1.055 mPas) of the 10 g/l V3 barely differs from the
viscosity of water, the permeability of the rock was 0.00633 mD, i.e. 6.33 D. From the above results the
permeability reduction effect in percentage can be calculated giving the data of: 90.028, 99.555 and
99.932% for P1 solution (core A), P2 solution (core B) and V3 solution (core C) respectively.
In the following step, the regainable permeability was determined, which can be characterized by the
return permeability after the reverse injection of 100 ml formation water. Based on the results (see Fig.
12 14) the measured regained permeabilities were 3.244, 0.693 and 1.749 mD for P1 solution (core A),
P2 solution (core B) and V3 solution (core C) respectively. From these data the calculated irreducible
return permeability damages were 81.740, 94.522 and 81.294% for P1 solution (core A), P2 solution (core
B) and V3 solution (core C) respectively.

SPE-174260-MS

13

The results of the filtration tests can be summarized as follows: all three additives decrease rock
permeability over 90%, moreover, the effect of both V3 and P2 essentially corresponds to total blocking.
In accordance with the research program, the photon correlation tests of 10 ml of effluent fluid samples
have also been performed. The gained mono-modal data, the average particle size by volume are
illustrated in Fig. 15. It can be stated that only the 500 nm size particles of dispersed material are
relatively mobile in the pore matrix and produced back by reverse water injection. In the samples of V3
solution, the average particle size after injection of 80 ml water increases gradually.

Figure 15The average particle size of additives in the fractions after reverse injection of water

It can be concluded that the back production of barrier forming particles cause some improvement of
the regained permeability. Starting out of the 4.5 m average pore size of the porous media and the app.
80% macro-porosity and the nearly 100% permeability loss cannot be interpreted if only the colloidal
dispersed part present in the solutions is considered to contribute. The adsorption and adhesion interaction
of the rock/additive and its irreversible character are decisive in permeability reduction.
Selection and characterization of core samples-II
For other series of filtration tests, lower permeability and lower mean pore size core plugs were selected.
The data of the core plugs used for the filtration tests at 30 C are shown in Table 4 5, while pore
size distribution data can be seen in Fig. 16 19.

Table 4 Mercury injection data of Core D

Hg injection results
Sample
Chord

S-1(A)
27.45

mm

7.017.45

mm

Cross section
Volume
Dry mass
Temperature

1.371
0.9612
2.3459
22.5

cm2
cm3
g
C

Maximum press.

3505.10

bar

(A)(B)

Complete injected
volume:
Complete specific
surface:
Average pore radius
(m):
Porosity:
Complete density.
Matrix density:
Macro porosity (up
to 2 bars)
Micro porosity lover
2 bars)

0.0620

cm3/g

06700

m2/g

3.7730

14.334
2.3127
2.6997
5.481

(%)
g/cm3
g/cm3
(%)

8.853

(%)

14

SPE-174260-MS

Table 5Mercury injection data of Core E

Hg injection results
Sample
Chord

S11 (B)
27.13

mm

7.287.40

mm

Cross section
Volume
Dry mass
Temperature

1.317
0.9745
2.4209
23.2

cm2
cm3
G
C

Maximum press.

3504.09

bar

(A)(B)

Complete injected
volume:
Complete specific
surface:
Average pore radius
(|im):
Porosity:
Complete density
Matrix density:
Macro porosity (up
to 2 bars)
Micro porosity (over
2 bars)

0.0565

cm3/g

1.0830

m2/g

1.3630

13.214
2.3384
2.6945
5.061

(%)
g/cm3
g/cm3
(%)

8.153

(%)

Figure 16 Pore size distribution data of Core #x201C;E#x201D;

Figure 17Pore size distribution data of Core #x201C;E#x201D;

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15

Figure 18 Differential pore size distribution data of Core D

Figure 19 Differential pore size distribution data of Core E

The common properties of absolute and differential pore size distribution curves is the deviation
resulting in a relatively large difference in the absolute permeability of the core plugs in spite of the
average size of pore radii being apparently close to each other (3.772 and 1.363 m). This is the result
of the significant difference in the range of relative pore size distribution (see Fig. 18 and 19).
Particle size measurements-II
Particle size distribution tests were performed with low-angle Back Scattering Laser Photon Correlation
Analyzer and Nanosizer at 25 C temperature for the following three solutions:
DF - dynamic filtrate of laboratory prepared HTHP drilling fluid formulation,
PO2 - same as the liquid phase of the said HPHT drilling fluid containing P1, P2 and V3 polymers and
filtered on PO2 glass filter (to remove large particles),
SF - same as the liquid phase of the said HPHT drilling fluid containing P1, P2 and V3 polymers and
allowed to settle and separate the lower dense phase (concentrating large particles in test fluid). The
particle size distributions of the solutions are illustrated in Fig. 20.

Figure 20 Particle size distributions by volume for DF, PO2 and SF fluids

The following can be concluded from the test results:

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1. All samples show multimodal (bi- or tri-modal) structure in the by-volume distribution curves. The
bi-modal structure is characteristic of the settled (SF) fluid sample.
2. Considering the mass and volume of the dispersed phase, the particle sizes of 25-35 nm, 100-160
nm and 500-800 nm are dominating the distributions. Surprisingly, a dispersed phase of 25-35 nm
size can not be observed in the settled sample.
3. The comparison of the fluids allows to conclude for sample SF, that the porous ceramic disk and
the filter cake partially retained the larger particles therefore the volume of the 100-160 nm and
500-800 nm fractions was smaller than in case of the PO2 sample (filtered on PO2 laboratory glass
filter).
4. The 25-35 nm peak is absent in the distribution curve concerning the settled (SF) fluid sample.
This indicates that during sedimentation this small sized material was trapped by the settling
particles and/or remained in the upper (lighter) phase.
5. Comparing the particle size distribution curves measured for the fluid (DF, PO2 and SF) samples
with the curves obtained for the aqueous solutions of P1, P2 and V3 additives, it can be stated that
they show a large-scale similarity. Resulting from this, the peaks characteristics of the filtrate can
be related to these materials.
Core flow test results, filtration study-II
The aim of these laboratory filtration tests was to determine how the injection of solutions filtered through
PO2 glass filter and sample of settled dispersed phase influence the permeability of the natural porous
system, and what return permeability characterizes the reverse injection of water. On core plugs cut from
expressly low permeability natural rock, the below injection protocol was conducted:
1. Saturation of the core plug with formation water,
2. Determination of balanced water permeability (injection of 4 PV of formation water),
3. Injection of PO2 and SF solutions (1 PV) and continuous determination of permeability,
4. Reverse water injection,
5. Continuous registration of water permeability and after injecting 5 PV of formation water,
determining regained permeability. The mobility values, calculated based on the measured data in
relation to the volume of the injected fluid can be seen in Fig. 21 and 22.

Figure 21Core flow test of PO2 glass filter filtrate (Core D)

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Figure 22Core flow test of settled sample (Core E)

Based on the data shown in Fig. 21 and 22 the water permeability of core samples were 1.9 mD and
0.19 mD for Core D and Core E respectively. The computation of permeability from mobility data was
performed assuming 10 mPas dynamic viscosity. Mobility was decreasing gradually and radically
during the injection of the filtrate (PO2 glass filter) and the settled (SF) fluid sample. At the end of the
injection of the 1 PV of these fluids, the mobility can be considered as zero on a linear scale.
The mobility on the logarithmic scale (Fig. 23 and 24) was 0.0006 mD/mPas (PO2 filtrate) and 0.0010
mD/mPas (SF settled) on Core D and Core E respectively. The blocking effect improved compared to the
before-mentioned minimum during the following water injection and set in the values of 0.300 mD/mPas
(PO2 filtrate) and 0.035 mD/mPas (SF settled) on Core D and Core E respectively. It was also interesting
that during reverse water injection the coloring (dark brown) material of the filtered sample (PO2) was
eluating from the core plug for a long time, while the settled (SF) sample resulted in a practically colorless
effluent after 2 PV.

Figure 23Core flow test of PO2 glass filter filtrate (Core D) (logarithmic representation)

Figure 24 Core flow test of settled sample (Core E) (logarithmic representation)

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SPE-174260-MS

This observation in addition to the data illustrated in Fig. 21 24 and compared to data for particle size
distributions shown on Fig. 20 clearly suggests that although classical pore plugging theory may not be
used for low pore size (i.e. in nano) ranges, certain fit of particle size distribution of filtration control
additives to pore size distribution is inevitable to achieve efficient pore blocking in low pore size range.
Data of Fig. 22 showing lower permeability reduction can be attributed to the absence of low size particles
in the settled fluid sample, supported by missing of coloring components. This fact also shows the
importance of blocking of very low size pores as well.
Particle size measurements for cloud-point-glycols
Polyalkylene-glycols (PAG) or so-called cloud point glycols (CPG) have been successfully used for shale
drilling from the early 90s all around the world (van Oort, 2003 and Bland et al., 1996). Recent
applications in Hungary also proved very good field results. The water-soluble PAG (low molecular
weight ethylene/propylene-glycol block copolymer) at elevated temperature clouds out of the drilling fluid
and forms solid-like particles. This temperature is called as CPT (cloud point temperature). As it is known
during drilling the circulated drilling fluid temperature in the bottom hole region can be by 30 - 60 C
below the formation temperature (depending on the actual formation temperature, geothermal gradient,
depth and flow rate). In a temperature window when the drilling fluid temperature is below and the
formation temperature is above the CPT the PAG being dissolved in the drilling fluid and enters with the
filtrate into the formation (into the shale pores) and clouds out from the filtrate, forming solid-like
particles in the pores and builds up a physical barrier that prevents further filtrate invasion. This
phenomenon of shale stabilizing mechanism is well understood in relation to efficient plugging of
nanosize pores (Relay et al. 2012).
The routine test for CPT of PAG is based on visual or photometric observation of change of
transparency of the PAG solution. Unfortunately slightly more than nothing is known about the structure
of PAG1s solution above the CPT. The interest was to know more about the particle sizes formed above
the CPT in order to have a better estimation of pore/fracture plugging/sealing potential and efficiency in
the presence of larger size openings.
Out of the large number of particle size measurement results only a few shall be used to highlight the
characteristic changes in particle size of 40 g/l PAG (industrial/commercial sample) dissolved in 20 g/l
K-formate solution. Results of particle size distribution measurements are illustrated in Fig. 25 27. Fig.
25 show certain amount of detectable particles well below the CPT. Getting closer to CPT larger size
particles are formed, the particle size distribution curve changes from mono-modal to bi-modal and clearly
indicates the forming of larger particles while smaller ones maintain their sizes (see Fig. 26).

Figure 25Particle size distribution below CPT

SPE-174260-MS

19

Figure 26 Particle size distribution approaching CPT

Figure 27Particle size distribution above CPT

Above the CPT the small particles disappear, the particle size distribution curve changes to multimodal
(see Fig. 27) with particle sizes between 400 - 1000 nm and 5 - 15 m. The data summarized in Fig. 28
referred to 40 g/l PAG dissolved in 50 g/l K-formate* solution shows similar picture with more complex
size ranges. Above CPT, the particle size distribution data obtained for PAG in brine system suggest
acceptable pore/fracture plugging/sealing capability in presence of larger openings.

Figure 28 Particle size distribution above CPT *

It was interesting (and surprising) to detect small size (30 -50 nm) particles far below the CPT. At the
same time this can be a practical and reliable explanation for recent field experiences with good
shale/wellbore stabilizing performance of PAG-polymer drilling fluid in upper borehole sections as well,

20

SPE-174260-MS

where the formation temperature was below the CPT. Laboratory tests performed with latex particles
virtually support this shale stabilizing effect (Liu et al., 2014).
It should be understood that although formation damage control during drilling operation is one of the
most important concerns in many complex situations a compromise with other technical issues must be
made. In recent experience a good example was shown how the formation damage (permanent permeability reduction) can provide (in compromise) technical benefits (Byrne et al., 2013). Based on
laboratory results and technical considerations this paper is intended to highlight that at difficult drilling
and complex geological conditions (e.g. unconventional resources) formation damage can be treated in
a different way. High filtration rate (liquid/solids invasion) into low pemeability formations causes
formation damage and simultaneously wellbore instability due to pore pressure penetration and changes
in rock mechanics (stress alteration, physical weakening by hydration, swelling, etc.). The objective was
to form a thin layered, ultra-low permeability physical barrier strictly in the near-wellbore region that is
targeted to control/prevent fluid and solids invasion deeply into the formation. This can serve to minimize
in-depth formation damage and wellbore instability potential. Due to the special drilling fluid flow,
conditions at bit the role of internal filter cake properties and conditions for its depositon become a priority
in selecting additives and design of drilling fluids. Such physical barrier, a properly designed and
deposited internal filter cake can fulfill several functions by minimizing, preventing further fluid invasion:
1. Minimizing in-depth permeability damage and rock/fluid interactions (fines migration, wettability
changes, stress changes, softening/weakening),
2. Maintaining near-wellbore pressure drop and wellbore pressure support, promotes wellbore
stability,
3. Minimizing drilling related problems (differential sticking, high torque, etc.),
4. Providing better conditions for reaching virgin rock surfaces by perforation.
Simulation and better insight into downhole filtration/invasion process and conditions are unavoidable
in estimation of drilling fluids solids/liquid invasion and related potential of near wellbore permeability
reduction (formation damage) and wellbore instability when drilling through low permeability (i.e.
unconventional) formations. Detailed study of all factors affecting internal filter cake buildup based on
realistic, complex downhole conditions are critical to achieve best performance of applied drilling fluids.
Buildup of a very low permeability (ideally impermeable), thin internal filter cake in close to the wall of
wellbore region serves as a physical barrier that essentially prevents (minimizes) solids/filtrate invasion
(minimizes in-depth formation damage) and prevents (minimizes) filtrate pore pressure transmission
(keeps wellbore pressure support and maintains wellbore stability). Lower volume of filtrate in the near
wellbore region can dissipate into the formation on a long-term basis opening the pore network toward the
wellbore.
Conclusions
Based on the discussed concerns and the results obtained in laboratory tests the following conclusions can
be drawn:
1. In low permeability formations due to low pore sizes the classic bridging theory (particle size
design) is practically not applicable therefore the fluid loss (filtration) control (and other special)
additives should be properly selected with special focus on nano-size particles.
2. For low permeability formations the drilling fluid testing and design should involve properly
designed core flow tests using individual additives and/or simulated (drilling fluids) liquid phase
in order to evaluate filtration control properties regarding to internal filter cake formation and
associated permeability reduction.
3. Particle size measurements in the nano-size range are essential (in addition to cores pore size
distribution and conventional PSD) in drilling fluids design.

SPE-174260-MS

21

4. The results of particle size measurements using Back Scattering Laser Photon Correlation
Analyzer and Nanosizer for three individual, polymeric (synthetic and natural) fluid loss control
additives in solution show different particle size distributions dominantly in the 20 - 1000 nm size
range and a theoretical combination of the three additives can provide well balanced coverage for
this size range.
5. Evaluation of particle size distribution data proves the aggregation tendency of the polymers. The
ratio of larger size gel particles formed as a result of intermolecular interaction is increasing with
increasing of polymers concentration.
6. Core flow tests using low permeability core plugs showed almost 100 % permeability reduction
after the injection of less than 1 PV polymer solution. This can be attributed to the pore plugging
effect of gel particles and adsorption/adhesion interaction with the rock. The results refer to
potential efficiency of such additives in forming ultra-low permeability internal filter cake. This
can be positively interpreted as the same polymers are field proven additives as HTHP fluid loss
agents (in forming low permeability external filter cake).
7. At the same time the pore plugging efficiency showed clear deficit in absence of small (100 nm)
particles (Fig. 21 and 22). Therefore it can be stated that proper fit of liquid phase solids particle
size distribution to pore size distribution is required to form low invasion, low permeability
internal filter cake.
8. Design of drilling fluids to be used for low permeability formations should involve the incorporation of small size (10 - 1000 nm) dispersed particles in proper concentration. Testing procedures
should be worked out for additives selection and appropriate performance tests.
9. Particle size measurements on cloud point polyglycol (PAG) below and above the CPT proved that
particles sizes between 400 - 1000 nm and 5 - 15 m were formed above CPT and those can
provide acceptable pore/fracture plugging/sealing capability from nano size pores to micrometer
size openings (pores, micro-cracks, micro-fractures).

Acknowledgements
This work was supported by HOST Ltd. Permission by HOST Ltd to publish this paper and encouraging
the innovative R&D work is gratefully acknowledged.

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