SPE-176991-MS

Novel Micro and Nano Particle-Based Drilling Fluids: Pioneering Approach

to Overcome the Borehole Instability Problem in Shale Formations
Jie Zhang, Long Li, Shuangwei Wang, Jianhua Wang, Henglin Yang, and Zhiliang Zhao, CNPC Drilling Research
Institute; Jinzhi Zhu, and Zhen Zhang, Petrochina Tarim Oilfield Company

Copyright 2015, Society of Petroleum Engineers

This paper was prepared for presentation at the SPE Asia Pacific Unconventional Resources Conference and Exhibition held in Brisbane, Australia, 9 11 November
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
Oil-based mud (OBM) has strong inhibitive ability, which can prevent shale formations from
hydration and swelling, and thus is often used in the development of shale gas reservoirs in China.
Due to the low formation temperature (under 90 C), high pressure (with pressure coefficient up to
2.2), long barefoot interval (up to 2138 m), borehole instability problem is easily encountered in
dealing with the drilling of horizontal intervals of shale gas wells, which brings great challenges to
drilling fluid technology.
Maintaining wellbore stability is the most critical aspect of drilling operations of horizontal well
intervals. However, most of OBM system can not prevent filtrate invasion into nano-sized pores and
micro-fractures on shale surface, and subsequent cause borehole instability problems. The main reason is
that conventional drilling fluid particles are too large to seal the nano-sized pore throats or micro-fractures
in shales, and thus can not stop fluid invasion. A new type of composite particles is developed, and the
mean particle diameter of composite particles is about 105.6 nm. These micro-nano particles (MNP) are
added to OBM, and their influence on shale stability is evaluated.
The core displacement experiment indicates that these micro-nano particles can reduce the shale
permeability by a significant amount, and thus stop fluid invasion and inprove wellbore stability. The
reason is that these particles are small enough to penetrate and seal the pore throats in shale, and built
an effective internal mud cake possessing low permeability on shale surface, resulting in the
reduction of filtrate penetration into the shale. The experimental results show that these particles can
prevent pressure transmission and improve wellbore strength greatly. In addition, MNP have no effect
on rheological properties of drilling fluids, and they are environmentally friendly, too.
As a result, MNP can reduce fluid losses to the formation significantly, and consequently provide
an excellent sealing effect, so MNP are an effective plugging agent for strengthening wellbore
stability. Reduction of fluid losses and enhancement of wellbore strength can be achieved by addition
of these micro-nano particles to oil-based drilling fluids. MNP-based drilling fluids have been
successfully run for dozens of wells in Weiyuan-Changning and Shaotong shale block. The field
2 SPE-176991-MS

application indicates that no borehole instability problems are encountered in the drilling process of
horizontal well intervals. Using these MNP-based fluids containing micro-nano particles to seal the
shale is a very powerful and economical approach to address borehole instability problem in
troublesome shale formations. These MNP-based fluids are suitable for the drilling of long sections
of horizontal laterals. In the future, the MNP-based drilling fluids might hold great promise to resolve
shale instability problem.
Introduction
Significant borehole instability problems have been encountering in the drilling process of extended-
reach wells with long open hole sections in Weiyuan-Changning Block and Shaotong Block in China.
The parameters of shale gas block in Sichuan province are shown in Table 1. Maintaining wellbore
stability is the most critical aspects of drilling operation of oil-gas reservoirs. But most of conven-
tional water-based mud can easily generate filtrate invasion into shale formations, and subsequent
cause borehole instability problems, resulting in wellbore collapse, borehole shrinkage, and pipe
sticking. The basic reason is that conventional fluid loss additives can not form effective mud cake
to plug nano-sized pore throats in shales, and thus do not stop filtrate invasion into formations.

Table 1the parameters of shale gas block in Sichuan province

Parameter Changning Block Weiyuan Block Shaotong Block

Porosity, % 2.9-5.0 2.4-4.87 2.4-5.6

Pressure coefficient 2.03 1.96 2.0
Clay content, % 25.2 31-45 27.5
SH-Sh, MPa 10-13 15-19 15-18
Friability index 55-65 46-69 47-75

In the current study, the multifunction of drilling fluid additives and novel environment-friendly
drilling fluid system are the new hotspot in this field. Micro-nano materials offer the promise of petroleum
development and production. Micro-nano materials have many unique characteristics, which can play an
active role in improving mud cake quality, maintaining borehole stability, protecting the reservoir, and
meeting the needs of drilling operations under complicated geological conditions. Micro-nano materials
have the potential of revolutionary impact in the fields of drilling fluids. Currently, Micro-nano materials
are considered to be the most promising matter of choice for design and development of novel drilling
fluids, and may offer a better solution to petroleum industry problems that cannot be solved with
traditional methods
A new type of micro-nano particles (MNP) is developed, and MNP-based drilling fluids are formed.
The results indicate that MNP-based drilling fluids can produce an ultra-thin, tight and relatively
impenetrable mud cake deposited on the borehole wall, and can reduce filtrate invasion into formations
and hence minimize fluid-induced damage. In addition, MNPs could also possess the small sized pores to
block throats and interact with the clay particles, and consequently provide an excellent sealing effect and
inprove wellbore stability.
Using these oil-based drilling fluids containing MNP to seal shale formations is a very powerful and
economical approach to address borehole instability problems in troublesome shale formations. As a
result, these MNP-based drilling fluids are suitable for the drilling of long sections of horizontal laterals.
In the future, these MNP-based drilling fluids might hold great promise to resolve shale instability
problems. In addition, the application of MNP-based drilling fluid might offer high potential for reducing
SPE-176991-MS 3

the differential pipe sticking in highly permeable formations, formation damage and contamination while
drilling, and also could enhance ROP in hard rock formations greatly, and thus lower drilling costs
significantly

Characterization of Shale Formation

Analysis of minerology of shale gas reservoir

The mineral composition of shale gas formations is charactered by X-Ray diffraction (XRD), as
shown in table 2. The experimental results demonstrate that the mineralogy of shale samples from
Weiyuan-Changning Block comsists of quartz, illite, calcite, dolomite, microcline, pyrite, illite/
smectite and chlorite. Remarkably, the shale samples contain a certain amount of illite and illite/
smectite.

Table 2XRD analysis on shale samples from Weiyuan-Changning Block

Minerology

Well Number Depth (m) quartz I/S illite kaolinite chlorite microcline calcite dolomite pyrite

Ning 201 2517 33.8 5.14 27.3 1.98 5.14 9.3 10.7 2.0 3.5
Ning 203 2300 29.6 6.36 35.2 2.44 4.89 6.9 9.0 2.3 2.7
Wei 201 2767 39.8 3.47 27.8 1.39 2.08 4.8 9.5 4.4 6.2
Wei 201 2671 27.6 1.28 21.8 1.02 1.54 4.3 21.6 14.8 5.4
Wei 201 2697 22.6 0.8 24.3 0.8 0.8 3.3 20.7 22.5 3.8
Wei 201 1452 41.7 0 14.4 0.3 0.3 3.9 23.2 9.0 5.8
Wei 201 1508 24.0 0.76 22.8 0.76 1.01 6.0 32.0 6.4 5.8

Meantime, the percentage of illite is within the range of 69% and 96%, and it is the main mineral
composition of shale samples. Illite is a kind of dispersive and non-swelling clay minerals. The shale
formations contain large amouts of quartz (its percentage is 24%~41.7%) and carbonate (calcite and
dolomite), resulting in high porosity and high permeability. There are small proportions of illite/
smectite (less than 5%), which is the primary cause of severe borehole instability problems by the the
swelling properties of smectite. Based on the analysis of shale mineralogy, the shale gas formations
in Weiyuan-Changning Block have a high content of non-swelling clay minerals. In addition, the
cation exchange capacity of shale samples is 5.17 mmol/100 g. Therefore, the borehole instability
problem is caused by dispersion of clay minerals rather than swelling of clay minerals.

SEM analysis of shale samples

The SEM images of shale sampls from Ning 203 well (2300.69-2301.01 m) and Wei 201 well
(2767.13-2767.31 m) are analysized, as shown in Figure 1. The experimental results indicate that the pores
of samples are between nanometer and micrometer. The diameter of large pores is around 200 nm, and
the average pore diameter is about 80 nm.
4 SPE-176991-MS

Figure 1Scanning electron images of shale samples from Weiyuan-Changning Block

Meanwhile, there are several microfractures in the shale samples from Ning 203 well, and the width
of microfractures reaches the micrometer grade. As a result, the shale gas formation of Wei 201 well is
a kind of tight reservoirs with large amouts of pore throats and microfractures.
Analysis of contact angle of shale samples
The contact angles of water drops and oil drops (kerosene) in the shale sample surface from Ning 201-H1
well are tested, as shown in Figure 2. The experimental results demonstrate that the oil droplets can
completely spread on the surface of shale sample. However, the water droplets show a measurable contact
angle. So the shale samples have good capacity of oil wettability.

Figure 2the wettability of water drops and oil drops on the shale samples from Ning 201-H1 well

According to the analysis of the physical and chemical properties of shale samples, the mechanism of
borehole instability could be concluded as follows:
SPE-176991-MS 5

1. Due to the fractures and microfractures on the surface of shale formations, the invasion of filtrate
or drilling fluids into the pores along the fractures will cause the increase of pore pressure. If
filtrate has invaded into all microfractures in the space around one broken fragment, it is possible
for broken fragment to loss the supporting role of pressure of drilling fluids, resulting in spalling
and caving.
2. Due to the capillary imbibition effect of shale pores, the pore pressure increases, causing
dispersion, spalling, and collapsion of mud shale. The capillary pressure can improve the capacity
of oil wettability of shale formation. Shale formation has many small pore throats with low
permeability. Based on Laplaces equation, these small pores with the average diameter of 5 nm
can generate a pressure of about 30MPa.
3. The invasion of drilling fluid or filtrate into the formation may lead to borehole instability. While
filtrate penetrates into the formation, the pore pressure on the borehole wall will increase gradually
with time. When the fluid column pressure is not sufficient to support the pore pressure, the stress
of wall rock on the borehole wall is bigger than the strength of the rock itself, borehole instability
is encourtered.
In addition, OBM system is recommended to drill the horizontal intervals of shale gas wells in recent
years. The microfractures of the shale formation will open when the filtrate invades into the formations
via capillary force and the pressure of drilling fluid column; and it is difficult to form mud cake on the
borehole wall because the diameter of pores in shale is too small. The key to solve borehole instability
problem is to prevent the liquid pressure transmission. Therefore, the sealing of the microfractures or
pores in shale formation on the borehole wall to stop the pressure transmission is the key for the
improvement of wellbore stability.
Research of MNP-Based Drilling Fluids
Drilling fluids characterization
Due to its inhibitive characteristics and superior lubrication characteristics in comparision with WBM,
OBM mud is used to drill the horizontal intervals of shale gas wells in recent years. The basic formula
of OBM formula is shown in table 3.

Table 3the basic formula of OBM

Oil/water ratio 95/5
Emulsifier 5 L/m3
Lime 15 Kg/m3
Gilsonite 20 Kg/m3
Organophilic clay 10 Kg/m3
Barite The density of mud is 2.0g/cm3

To seal the microfractures or pores on shale formations, a new kind of micro-nano particles (MNP) is
prepared and then is mixed with glide graphite for enhancing lubricity. Graphite with the concentration
of less than 0.5 wt% is added to MNP, because the graphite with the concentrations of more than 0.5wt%
will give a precipitate while they are mixed with MNP.
The properties of MNP-based drilling fluids
The mixing formulas and rheological properties of MNP-based OBM formulas are shown in table 4 and
table 5. Table 4 presents the test matrices, which illustrates the nomenclature used to simplify the mixing
formulas. From table 4, the expression GF stands for drilling fluid formula added by MNP and 0.5 wt%
graphite. The expression NF is used to indicate drilling fluid formula only added by MNP. Table 5 shows
the rheology parameters of all drilling fluid formulas.
6 SPE-176991-MS

Table 4 the mixing formulas of graphite and micro-nano particles

MNP

Composition 0.5% 1.0% 2.0%

Graphite 0% NF1 NF2 NF3

0.5% GF1 GF2 GF3

Table 5the properties of OBM formulas

Composition (g/cm3) PV (mPa.s) YP (Pa) GEL (Pa/Pa) ES (V)

CS 2.0 32 4 1.5/2 2000

NF1 2.0 33 3 2/3 1998
NF2 2.0 31 3 2/3 2001
NF3 2.0 33 3 1.5/2 2000
GF1 2.0 39 4 2/3 1997
GF2 2.0 40 5 2/4 1999
GF3 2.0 37 5 2.5/4 2000

Compared with CS, the plastic viscosity and the yield value of NF-based drilling fluid hasnt changed
very much, In general, the rheology was not significantly affected by the addition of MNP. Moreover, the
addition of MNP to drilling fluid formulas has no influence on the emulsion breaking voltage of drilling
fluids. Remarkably, MNP have little effect on rheological properties of drilling fluids, and graphite does
not have a great impact on the rheological properties also.
Analysis of size distribution of NMP
Figure 3 shows the size distribution of NMP. The medium diameter of MNP is about 0.1056 m, D10
is 0.0667 m, D50 is 0.1061 m, D90 is 5.538 m, which belongs to the range of nanometer and
micrometer grade. The size of lager-sized particles is about 1/3~2/3 of the microfracture diameter of
the wellbore, so lager-sized particles will easily bridge and plug within the formation in the course
of spurt loss of drilling fluids. The size of smaller-sized particles can enter the pore throat on the
surface of borehole wall, and form tight and thin internal mudcake, resulting in wellbore strengthing
of shale formation.

Figure 3the size distribution of NMP

SPE-176991-MS 7

Core displacement experiment

Core displacement experiment is conducted by testing the permeability and permeability recovery of
low permeability cores contaminated by MNP-based drilling fluid in comparison with drilling fluid
formula without addition of MNP. The displacement pressure curve of drilling fluid formula without
MNP is shown in Figure4(a). The maximum displacement pressure is about 0.65 MPa in the process
of positive displacement before contaminated by oil based drilling fluid, and it is about 4.3 MPa after
contaminated by OBM formula. However, the maximum displacement pressure of reverse displace-
ment process is about 0.6 MPa.

Figure 4 the core displacement curve of various oil-base drilling fluid formulas

The displacement pressure curve of MNP-based OBM formula is shown in Figure 4(b). The
maximum displacement pressure is about 0.6 MPa in the positive displacement before contaminated
by OBM, and the maximum positive displacement pressure can reach up to above 19 MPa after
8 SPE-176991-MS

contaminated by OBM, but the maximum displacement pressure in the process of reverse displace-
ment is about 0.5 MPa.
In addition, the permeability recovery can reach up to 99.6% after adding 1 wt% MNP to oil-based
drilling fluid formula, and the plugging rate is close to 100%, so MNP compound have excellent
sealing ability. The core displacement experiment indicates that these micro-nano particles could
reduce the shale permeability by a significant amount, and thus stop filtrate invasion into shale
formation and inprove wellbore stability. The reason is that these particles are small enough to
penetrate and seal the pore throats and microfractures in shale formation, and build an effective
internal mud cake possessing low permeability on shale surface, resulting in the significant reduction
of fluid penetration into the shale.

Filter loss experiment

Table 6 shows the thickness of filter cake formed by various OBM formulas. The percentage of filter loss
reduction of MNP -based mud of different concentrations under LPLT API standard test at 30 min is shown
in Figure 8. The percentage is calculated on a basis of fluid loss of conventional plugging agent such as LCM.
Every experiment is repeated by three times and the standard deviation is shown for each point. The effect of
MNP on the filtration of drilling fluids is evaluated in comparison with drilling fluids without addition of MNP
and graphite. The filtration value of OBM formula is reduced significantly when 1wt% MNP is added to
drilling fluids.

Table 6 the thickness of mud cake and filter loss of various OBM formulas
Thickness of mud cake (mm) Filter loss (mL)

Composition API HTHP FLAPI FLHTHP

CS NPT 1.90 1.82 10 7.4

90C, 16h 0.48 4
NF1 NPT 1.70 3.22 7 3.4
90C, 16h 0.80 2.8
NF2 NPT 1.28 1.16 6.2 3.2
90C, 16h 0.72 2.4
NF3 NPT 1.08 2,44 4.8 2.4
90C, 16h 0.62 2
GF1 NPT 1.74 2.76 7.4 3
90C, 16h 0.66 2
GF2 NPT 1.54 2.32 7.2 2.8
90C, 16h 0.62 1
GF3 NPT 1.10 2.16 5.8 2
90C, 16h 0.50 0.8

Figure 5 shows the percentage of reduction of mud filtration when MNP and graphite are added to base
drilling fluid formula. The fluid loss of base drilling fluid formula is 7.4 mL at 30 min. The maximum
percentage of mud filtration is about 67% at the highest concentration of MNP. The reason for this is that
MNP can enter the pores of filter paper to reduce filtration. The drilling fluid formulas added by an
appropriate level of 0.5 wt% can be beneficial for the reduction of filtration especially when the
concentration of MNP is more than 1 wt%.
SPE-176991-MS 9

Figure 5Percentage of reduction of filtration at 30 min under HTHP conditions

MNP work better at high concentrations in contrast to what is observed at LPLT, but bigger filtration
reduction is obtained at low concentrations. MNP have an effect on filtration reduction in comparison to drilling
fluid formulas without MNP. The HTHP and LPLT experiments of MNP are conducted by three times for each
concentration. For MNP, the addition of 0.5 wt% graphite to drilling fluid can have a positive effect on the
filtration reduction, mainly because of the interaction of MNP and graphite at HTHP conditions. MNP with the
concertration of 2.0 wt% is observed to be the optimum concertration. Therefore, the filtration control
properties of mixing formulas of MNP and graphite are better than MNP at HTHP conditions.
The thickness of filter cake after 30 min for each experiment is shown in Figure 6. Compared with
drilling fluid formulas containing MNP, OBM formulas containing no graphite have an average increase
of 45%, and OBM formulas containing 0.5wt% graphite have an increase of nearly 30%.

Figure 6 (a) Filter cake formed by OBM formulas containing MNP at HTHP conditions; (b) Filter cake formed by OBM formulas
containing MNP and 0.5 wt% graphite at HTHP conditions
10 SPE-176991-MS

Figure 7 shows the relationship between the increment of filter cake thickness and the concentration
of MNP at HTHP conditions. This plot is constructed on the basis of average thicknesses of filter cake.
At high concentrations of graphite there is a slight effect on the concentrations of MNP. However, the
thickness of filter cake will increase greatly when OBM formula is not added by any graphite. This
significant increase of filter cake thickness is due to the filtrate being not effective at high concentrations
of graphite at HTHP conditions.

Figure 7Filter Cake thickness increment vs. MNP concentration

Field Application of MNP-based OBM

The field test of MNP-based OBM in YS 108H3-1 well

YS 108H3-1 well is a horizontal shale gas well located in Sichuan province. Its horizontal section
length is as high as 1532 m, the pressure coefficient can reach up to 2.0, and the bottom hole
temperature is 90 C. The horizontal section is drilled using OBM system. As the mud density reaches
2.0 g/cm3, the pump displacement should be 28 L/s to match rotary steering drilling system, so the
pump pressure is too high. The bottom hole temperature is about 90 C, so conventional fluid loss
additives such as asphalt compound can not have good filtration properties and sealing ability under
90 C. MNP-based OBM system is developed to solve the borehole instability problem in the process
of drilling operation.
The field application indicates that the rheological properties of MNP-based OBM system remain
stable at HTHP conditions. The rheology of MNP-based OBM is shown in Figure 8. After
MNP-based OBM system has been run for 30 days, it still has good comprehensive performance, and
borehole instability problems such as hole collapse and stuck pipe are not encountered, resulting in
the remarkable improvement of wellbore stability. Therefore, the stability of borehole wall can be
maintained by adding MNP compound to OBM to enhance the sealing performance of drilling fluids.
SPE-176991-MS 11

Figure 8 the on-site MNP-based OBM system

Application effect evaluation of MNP-based drilling fluid system

MNP-based drilling fluids can provide excellent fluid stability and rheology under HTHP conditions,
withstand high solids loading and deliver good sealing ability to microfractures or pores, as shown in table
7. The viscous shearing and solids content of MNP-based drilling fluids can always be kept in perfect
range, so the cuttings carrying efficiency could be enhanced and borehole cleaness could be improved.

Table 7the performance of MNP-based drilling fluids

Well Number Density, g/cm3 FV, s AV, mPa.s PV, mPa.s YP, Pa GEL, Pa/Pa HTHP, mL S, %

Well C 2.0-2.1 45-65 52-63 44-51 10-14 4-6.5/6-8 1-2.7 37-41

2.1-2.23 55-75 58-79 50-65 11-15 4-6.5/6-8 1.2-2.8 41-49
Well D 2.0-2.05 70-80 44-73 34-60 10.5-13 6-8/9-10 5-10 -53
Well E 2.0-2.06 60-80 60-80 53-70 7-11 4-6/8-12 2.2-3.0 -45

MNP-based drilling fluids have been recommended to run for dozens of wells and over 300,000 ft in
this block, as shown in table 8. The field application results indicate that the maximum mud density is 2.23
g/cm3, the maximum bottom hole temperature is up to 180 C, the maximum length of barefoot interval
is 2138 m, and the maximum burial depth of formation can reach up to 5700 m.

Table 8 the applied statistics of MNP-based drilling fluids

Block Base oil The amount of applied well
Chang Ning White oil 4
Fu Lin Diesel 48
Huang Jinba Diesel 2
Four record
Items Parameter Well
Max density (g/cm3) 2.2 YS108H3-2
Max temperature (C) 180 Shun nan3
Longest barefoot interval (m) 2138 Jiaoye12-4HF
Deepest depth(m) 5700 Dingye-2HF

While horizontal well intervals are drilled using MNP-based drilling fluids, the wellbore stability can
be maintained, and well-regulated borehole can be achieved, as shown in Figure 9. The returning cuttings
of shale formation are shown as Figure 10. The returning cuttings is regular, and clear cutting teeth marks
could be found, which indicates that MNP-based drilling fluids system has good inhibitive ability under
high temperature and high pressure conditions.
12 SPE-176991-MS

Figure 9 The caliper logging curves of horizontal well intervals drilled using MNP-based system

Figure 10 the returning cuttings of shale formations

Conclusion
1. The sealing of the micro fractures or pores on the borehole wall of shale formations to prevent the
pressure transmission is the key to the improvement of wellbore stability and well-regulated
borehole.
2. A new kind of micro-nano particles (MNP) is prepared, and it could plug the micro fractures or
pores on the shale formations effectively.
3. The MNP-based drilling fluid system has excellent rheological properties, good mud filtrate
control capacity and sealing ability under HTHP conditions, and it can meet the requirement of
drilling engineering of shale formations.
4. The MNP-based drilling fluid technology can solve borehole instability problem effectively, and
no pipe stuck event or other incidents related with drilling fluids is encountered, achieving safety
drilling operation.
SPE-176991-MS 13

Acknowledgements
The authors would like to thank the management of CNPC drilling institute for permission to publish this
paper and the operators who utilized the MNP based drilling fluids systems on shale blocks.

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