Journal Pre-proof

Pore-scale analysis of formation damage; A review of existing

digital and analytical approaches

Mahmoud Rezaeizadeh, Seyed Hasan Hajiabadi, Hamed Aghaei,

Martin J. Blunt

PII: S0001-8686(20)30614-X
DOI: https://doi.org/10.1016/j.cis.2020.102345
Reference: CIS 102345

To appear in: Advances in Colloid and Interface Science

Revised date: 10 December 2020

Please cite this article as: M. Rezaeizadeh, S.H. Hajiabadi, H. Aghaei, et al., Pore-scale
analysis of formation damage; A review of existing digital and analytical approaches,
Advances in Colloid and Interface Science (2020), https://doi.org/10.1016/
j.cis.2020.102345

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Pore-scale analysis of formation damage; a review of existing digital and

analytical approaches
Mahmoud Rezaeizadeh1, Seyed Hasan Hajiabadi1*, Hamed Aghaei2*, Martin J. Blunt3
1. Department of Petroleum Engineering, Hakim Sabzevari University, Sabzevar, Khorasan Razavi, Iran.

2. Petroleum Engineering Department, School of Chemical and Petroleum Engineering, Shiraz University, Fars, Iran.

3. Department of Earth Science and Engineering, Imperial College London, London, UK.
*
Corresponding authors: Seyed Hasan Hajiabadi (Email: [email protected]); Hamed Aghaei
(Email: [email protected])

Abstract

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Formation damage is one of the most challenging problems that occurs during the lifetime of a

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well. Despite numerous previous studies, an organized review of the literature that introduces
and describes the digital and analytical approaches developed for formation damage analysis is

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lacking. This study aims to fill this gap through briefly describing the main mechanisms behind
formation damage in porous media as well as investigating the main related experimental
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methods with an emphasis on novel imaging techniques. Specifically, there will be a focus on a
number of modern and nondestructive analytical methods, such as dry/cryogenic Scanning
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Electron Microscopy (SEM), X-Ray Diffraction (XRD), CT-scanning (both using adapted
medical scanners and the use of high-resolution micro-CT instruments) and Nuclear Magnetic
Resonance (NMR), which obtain outstanding results for the identification of formation damage
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mechanisms. These approaches when used in combination provide a robust identification of

damage processes, while they reduce the risk of operational mistakes for decision makers
through visualization of the distribution, severity, and nature of the damage mechanisms.
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Keywords: Formation Damage; Electron Microscopy; XRD; Computed Tomography; NMR.

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1. Introduction

Formation damage – an adverse change to the pore space of the reservoir rock during oilfield
operations – is well-known as one of the most serious issues in the oil and gas industry. The
damage is an end product of several mechanisms including physical, chemical, hydrodynamic,
thermal, mechanical and biological damage which are triggered during drilling, production,
workover, and hydraulic fracturing operations [1-3]. However, regardless of the reason, this
phenomenon can cause changes in pressure, sand production, scale precipitation, pore blockage,
and reduction in production rates below the expected economic limits [4, 5], and lead to a
reduction of production rate [6, 7]. Furthermore, damage may also limit the ability to inject fluids
of different composition into the formation.

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In extreme conditions, formation damage might even force well abandonment, especially in the
case of reservoirs with extremely low absolute permeability [8, 9]. In any event, damage imposes
extra costs related to well stimulation operations, and puts the economic validity of a well under
question due to a significant reduction in the well flow rate [10, 11].
During the last few decades, the above-mentioned consequences of formation damage have
inspired the development of experimental and analytical methods for understanding, preventing
and/or controlling formation damage in oil- and gas-bearing formations. In this regard,
laboratory experiments are crucial to replicate downhole operating conditions and to help
benchmark and validate numerical simulation models [3, 12, 13]. In addition, analytical
techniques provide quantitative measurements of the severity of damage and to suggest
procedures to prevent or reverse the reduction of reservoir deliverability avoiding further

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complicated expensive stimulation operations [14, 15].
Traditionally, core flood measurements are used to quantify the reduction in permeability. These

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averaged measurements can be complemented by optical petrography, Scanning Electron
Microscopy (SEM), X-ray Computed Tomography (CT) scanning, and Nuclear Magnetic

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Resonance (NMR) T2 relaxation measurements to identify the mechanisms of formation
damage, from which methods to avoid or reduce the damage can be designed [16-19].
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Each of these methods have their own advantages and disadvantages, both scientific and
economic. In the end a combination of techniques are needed for a full understanding of
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formation damage, with recent advances in imaging technology offering considerable promise.
Despite the numerous studies carried out in this field, there exists a lack of an organized
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introduction to the existing formation damage analytical approaches. The present work aims to
fill this gap through listing the major mechanisms contributing to formation damage phenomena
as well as the most common applied analytical methods, especially recently-introduced imaging
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approaches.
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2. Formation damage mechanisms

Drilling fluid invasion is considered as the first initiator of formation damage that plugs the pores
around the wellbore and is usually difficult to be removed using the back flow method [1]. The
magnitude of damage depends on a range of parameters including incompatibilities between
drilling fluids and formation water, exposure time of drilling fluids, and the amount of mud
filtrate leakage [20]. On the other hand, the accompanying solid particles may also cause
significant damage depending on their size distribution, formation pore distribution, and pressure
condition inside the wellbore [21].
In addition, the vast majority of natural damage leads to a severe reduction in reservoir
productivity [22]. For instance, deposition of paraffins and asphaltenic parts of the crude oil

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might take place in the wellbore, near wellbore zones, production equipment, perforation
channels, and producing slots [22, 23].

Moreover, a permanent reduction in permeability is expected during secondary recovery

processes mainly due to scale deposition resulting from incompatibility between formation water
and injected fluids, as well as organic precipitations formed by variations in thermodynamic
conditions [24, 25]. Fines migration is another drastic damage resulting from the injection of
high pressure fluids into the reservoir [26]. In addition, pore blockage in oil-bearing layers
caused by the retention or adsorption of chemicals flooded within reservoirs is another
significant cause of formation damage impeding the effective flow of chemical solutions, mainly
including polymers, surfactants, and nanoparticles, inside the porous medium which leads to
lower ultimate recoveries [5, 27].

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Table 1 lists the most common upstream operations, their possible associated damage and the

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potential prevention or remediation approaches.

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 Table 1. List of the most common operations in upstream oilJournal Pre-proof
and gas industry, associated formation damage and prevention/remediation approaches.

Operation Main damage mechanisms/effects Prevention / Remediation

 Air and/or gas drilling [28]

 Solid/fluid invasion [1]  Bridging material [32, 33]
 Absolute permeability reduction [1, 28]  Filter-loss control agents (such as organic oil-soluble particles) [21]
 Pore plugging [1, 29]  Water-based muds (WBMs) with divalent ions such as Ca2+ and Mg2+ [21]
Drilling  Emulsification [28, 30]  Perforation [2]
 Clay swelling [1, 22]  Dissolving the fines and enlarging the pore-throat sizes using acidizing and
 Dispersion and precipitation of salts [1] stimulation processes [2, 34]

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 Increased interstitial water content [28]  Using inorganic salts such as NaCl, KCl, NH4Cl, and CaCl2 in drilling fluids
 Fines migration and sand production [25, 31] (known as stabilizers) [35]

Casing and
 
 Nanofluids [36-38]

o o
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Hydration of cement [21] Addition of KCl to spacer or cement slurry [20]
Cementing
 Recreation of lime [21]  Fluid loss additives (such as HEC4 & PVA5) [20]

 Fresh water invasion [22]


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Open hole completion with gravel pack [40]
Completion 

Clay swelling [22]
Clay migration [22]
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

 eUnderbalance perforation [21]
Using clean perforating fluids [21]
Adequate shot density [21]



Water blocking [39]

Detrimental byproducts of stimulation [11]

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
Negative pressure completion (especially in perforation) [41]
HCl/HF solutions (with HBF4 [44], H3PO4 [45], AlCl3 [46], H3BO3 [46] or

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Stimulation
 Iron precipitation (due to acidizing by HCl) [42] CH2O2 [47])
 

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Permeability alterations [43] Using water- soluble polymers in fracturing fluids [48]

Primary



Blocking the pore throats [22, 23]

u r
Altering the formation wettability from water-wet to oil-wet [23]
Increasing hydrocarbon viscosity by nucleating water in oil
 Acidizing [49]

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 Injection of organic aromatic solvents and soaking [22, 23]
production emulsions [22, 23]
 Acid/solvent washes (for scale removal) [22]
 Permeability reduction [23]
 Sand control (in case of fines migration) [50]
 Plugging the production sluts and gravel pack [22]
 Inorganic scale [22, 25]
 Incompatible fluids [24]
 Suspended solids [21]
 Mineral scale formation [24]  Squeeze inhibitor treatment [24]
Water flooding  Permeability reduction [24]  Keeping a constant temperature [24]
 Bacterial problems [21]  Filtration [21]
 Fines migration [51]  Using nanofluids (such as SiO2) to prevent from fines migration [51]
 Microbial problems (like hydrogen sulphide gas by sulphate
reducing bacteria (S.R.B.)) [52]
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3. Formation damage analysis approaches

This section describes the standard traditional and modern analytical methods used to analyze
various kinds of formation damage.

3.1. Traditional analytical methods

Darcy’s law and thin section petrography (TSP) are among the two main traditional
approaches used for the evaluation of formation damage as discussed below.

3.1.1. Darcy’s law

Darcy’s law is used to measure the permeability of core samples before and after damage.
Here, core permeability can be determined using the linear relationship between the injection

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rate and the pressure difference across the core sample.

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One of the main disadvantages of this method is fulfilling the principle of steady-state
conditions, such that there are no changes in the core during the injection test. Reaching
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steady state may be impossible to achieve, as damage continues, or takes a long time. Also,
for tight samples, the relatively high displacing and confining pressures required might result
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in a low measured permeability caused by unavoidable changes in the stress state which
compress the rock. Consequently, the use of Darcy’s law is considered as impractical and
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inaccurate to evaluate damage in shales and tight sandstones [53]. Moreover, the difficulty of
relating the results to well inflow performance is a frustrating aspect of this method [9].

3.1.2. Optical Petrography (OP)

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This technique includes microscopic analysis of a rock thin section, typically around 30 µm
in thickness, which aims to describe various petrographic parameters including texture,
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fabric, sorting, primary and secondary porosity, fracture types, relative abundance, clay
minerals, and cementation [3]. However, detection of fines invasion and alteration of the pore
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structure can be challenging and the information provided by this destructive technique is
only applicable for samples for which thin sections can be acquired without altering the pore
space [54].

Li and He [55] employed the OP method to analyze the interactions between filter cakes and
rocks. They stated that thin section analysis can supply an appropriate means of assessing the
formation damage mechanism, and can be considered as a pragmatic tool for the evaluation
of drilling-fluid-based damage, particularly the effects of particle settling.

It is worth noting that, considering the recent developments in imaging techniques, OP is

mainly used in preparation for other analytical methods, such as X-ray CT scanning, SEM
and TEM, which are described next.

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3.2. Digital Rock Physics (DRP)

During the last decades, novel non-destructive imaging techniques and associated analysis
and modelling, often called digital core analysis or digital rock physics, have transformed our
understanding of processes in porous media [17, 56].

Three-dimensional (3D) imaging technology can be used to describe the nature and geometry
of mineralogical components while, along with 2D optical identification (see the previous
section), it can be used to identify organics in porous media [57]. However, 2D images alone
represent a biased perspective of the pore structure and cannot assess the connectivity and
hence permeability of the sample [56].

Inevitably there is a trade-off between the high resolution and ease of interpretation of 2D

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imaging methods – both optical and using electron microscopy – and the superior assessment
of connectivity, but with generally lower resolution achieved by non-destructive 3D X-ray

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imaging methods [54]. We will now present the different methods and assess their strengths
and weaknesses for the evaluation of formation damage.
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3.2.1. Electron microscopy techniques
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The wave characteristic of electrons was first theorized by Louis de Broglie in 1925.
Subsequently, in 1932, Knoll and Ruska proposed the idea of an electron microscope to
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compensate for the limited image resolution in optical microscopes [58]. The resulting image
could reach a 0.05 nm resolution and magnifications of up to about 10,000,000x mainly due
to the fact that electrons have de Broglie wavelengths of about 100,000 times shorter than
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visible light [59, 60].

3.2.1.1. Transmission Electron Microscopy (TEM)
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The first commercial TEM was developed by Metropolitan-Vickers Company, UK in 1936

that was also a trigger in outlining the idea of a practical electron microscope. Further
developments in the technology led to high-resolution transmission electron microscopy
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(HRTEM) [58].
TEM is acknowledged as a promising method providing accurate information on
crystallography, microstructure, and composition of the regions of micrometer to sub-
nanometer sizes in thin samples [61].
As an example of a recent application, Khishvand et al. [62] have demonstrated significant
fines mobilization during low-salinity water flooding using TEM to image effluent samples at
nanometer resolution (ranging from 0.28 to 9.9 nm). For instance, the TEM images in Figure
1 evidence the presence of grain (possibly clay) particles in low-salinity water flooding and
effluent samples with oil films adhered to their surfaces.

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Figure 1. (Top row) TEM images of the effluents of the HSWF (high salinity water flooding) experiments;
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(Second and third row) TEM images of the effluents of the LSWF (low salinity water flooding)
experiments [62].

3.2.1.2. Scanning Electron Microscopy (SEM)

SEM provides magnified images that help to reveal microscopic-scale information on the
size, shape, composition, crystallography, and other physical and chemical properties of a
specimen [63]. It was developed by German physicists in the early 1900's in parallel to the
development of conventional TEM [64]. The key advantage of SEM over TEM is that thick
samples can be used, as the electron beam scans the surface – the beam does not have to pass
through the sample to acquire an image.

Without any doubt, SEM plays a key role in various geological and petroleum engineering
fields, including pore-scale and invasion analysis, sediment diagenesis, mineral alterations,
texture and pore space properties, and the evaluation of fluids performance [65, 66]. In

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particular, SEM analysis can produce high-quality images of porous media even from low
permeability reservoirs [17, 57]. Moreover, combined with 3D image analysis techniques, it
has been widely used for qualitative analysis of formation damage [9, 67]. We now list some
of the more important studies which have studied the different chemical, physical and
biological processes causing formation damage.

Pittman and Thomas [68] discussed the applications of SEM to study reservoir rocks,
including for clay minerals and the formation damage they can cause. Later, Yang and
Sharma [69] employed this method to study the growth of large calcium carbonate or calcium
sulfate crystals in the pore space, as well as the presence of other fines in a sandstone core
invaded by cement filtrate.
Lappan and Fogler [70] studied the effect of bacterial polysaccharide production on

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formation damage and found evidence of bacterial plugging of the pores using the SEM
imaging technique. In another study, Ghalambor et al. [71] investigated the nature of

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formation damage due to the growth of bacteria on formation minerals. They confirmed the
growth of bacteria on the minerals and consequent reduction in permeability.
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Merdhah and Yassin [72] investigated the permeability reduction due to scale formation and
deposition during water injection where they employed SEM imaging to determine the
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particle size, morphology and formation of CaSO4, SrSO4, and BaSO4 precipitates.
Leontaritis et al. [73] presented an approach for prevention and treatment of formation
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damage caused by asphaltene deposition using thin section and SEM analysis. Moreover,
Arciniegas and Babadagli [74] used FIB-SEM to characterize the thickness of organic
deposition (mainly asphaltene and resins) on the surface of glass beads.
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Fraser et al. [75] used SEM and ESEM (Environmental SEM) to investigate the formation
damage characteristics of Mixed Metal Hydroxide (MMH) drilling fluids and compared the
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results with the ones achieved from polymer-based fluids. They used the ESEM in early tests;
however, due to the comparable results and the greater clarity of conventional SEM, ESEM
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was not used further for illustrative work. According to the results of SEM analysis, no
external cake was visible in the case of the polymer/KCl fluid and the SEM showed solids
invasion to around 200 µm depth following the formation of an internal cake.
Note that ESEM is an extension of the SEM method in which some of sampling preparations
and handling requirements for SEM are eased to provide a broader range of observation
conditions, especially for non-solid materials. SEM and ESEM are quite similar from a
hardware perspective. The main difference is the introduction of gases into the specimen
area of ESEM which aims to mitigate the charging effects in insulators, to provide an
alternative mechanism for amplification of electron signals, to examine the surface of
practically any specimen (wet or dry, insulating or conducing), and finally, to provide direct
observation of hydrated/liquid specimens in their natural state [76, 77].
Byrne et al. [78] presented the application of dry SEM and thin section analyses to determine
solid damage mechanisms, such as, clay fines migration, scale precipitation and drilling mud
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solids invasion. Moreover, they investigated the other types of formation damage, such as
wettability alteration, microemulsion-related damage, fluid retention, and oil or water
blockage using cryogenic SEM analysis. Furthermore, the study introduced a new technique
of cryogenic SEM using EDS (Energy Dispersive X-Ray Spectroscopy) analysis for X-ray
mapping of the remnant mud bodies to determine solid and fluid distributions.
Later, Sánchez et al. [79] performed a study on the behavior of scleroglucan-based
formulations generally proposed for high-temperature zones and/or high permeability
reservoirs against the more common xanthan-containing polymer flooding. Here, the cryo-
SEM dynamic filter-cake observations evidenced a lower filter-cake permeability obtained
under dynamic conditions with homogeneous structure, no aggregates, and a structural
polymer network.

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Schembre and Kovscek [80] used SEM to analyze the composition of selected effluent
samples to explain the mechanism of fines migration at elevated temperature that confirmed

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the production of fine clay material.
In another study, the evolution of sand pack pore and grain structure was determined using
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SEM imaging and compositional analyses where it was shown that hot alkaline water injected
at rates close to field rates resulted in grain-cementing precipitation [81].
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Habibi et al. [82] studied the use of different types of nanoparticles (NPs), including MgO,
SiO2 and Al2O3, to reduce fines migration in synthetic porous materials where SEM imaging
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was carried out for qualitative observation of fines attachment to pore surfaces. This work
clearly showed the adsorbed fines on the treated solid surfaces (Figure 2). The results suggest
the MgO modified nanofluid as the most efficient one to treat synthetic porous media.
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Figure 2. (Left) Fines attached on glass-beads surface without any treatment; (Right) attached fines on
treated glass beads with MgO [82].

Laboratory experiments were conducted by Tang et al. [83] to evaluate formation damage
caused by complete water vaporization and salt precipitation in sandstone reservoirs where
SEM imaging was used to observe the presence of crystal salts in pore throats. In particular,
SEM analysis suggested that the treated core inter-granular pores were filled mainly with
NaCl crystals causing blockage of the small pore spaces.

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Kar et al. [84] investigated the effect of various types of clay minerals on the performance of
Steam-Assisted Gravity Drainage (SAGD) where the SEM-EDS technique was used to study
the structural, elemental and petrophysical changes during the process.
Zhang et al. [85] took SEM images to study the texture of the fines generated from the shale
fracture face where the results showed that clay content in shale rocks is the fundamental
cause for the significant reduction of fracture conductivity after water flow.
Later, Xu et al. [86] reported the application of SEM imaging to investigate the effects of
formation damage on microscopic features of surface morphology in low permeability
reservoirs. The results not only showed changes in surface structures but also contributed to
better understanding of the Specific Surface Area (SSA) and Pore Size Distributions (PSDs).
SEM-EDS imaging was also employed to study the effect of mud weight on filter cake

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properties by Fattah and Lashin [87] where a greater reduction in permeability of the filter
cakes derived with the fluids treated with barite was observed compared with the ones treated

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with calcite.
Later, Yao et al. [88] employed SEM to distinguish and analyze micromorphological and
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geometrical features of the fines generated from tectonically deformed, undeformed and
granulated coal horizons.
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Rabbani and Salehi [89] presented a dynamic model for deposition of mud solid particles
over and through the porous sandstones during permeability plugging experiments where
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SEM coupled with image processing were used to find the porosity and pore size distribution
of mud cake.
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Table 2 presents a list of previous work, not already discussed above, on the application of
SEM in formation damage analysis in chronological order. The overall conclusion of this
section is that SEM techniques are widely used to study the nature of formation damage, as
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well as the composition and structure of effluent from damaged rocks.

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Table 2. A list of previous work on the application of SEM in formation damage analysis (sorted in chronological order).

Authors Method(s) Aim(s) Major achievement(s)

Combination of SEM with fluid loss analyses resulted in a

Hartmann et To analyze the original structure of drilling fluid filter cake through frozen-
SEM better understanding of formation damage and the principles
al. [90] hydrated and freeze-dried stages combined with the study of fluid loss data.
behind the creation of filter cake.

Argillier et
Cryo-SEM
Cryo-SEM-based characterization of mud cake structure achieved from
o f Correlation of internal and external structural characteristics of
al. [91] water-based drilling fluids with new formulas.

r o filter cake.

Merdhah and
SEM
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To analyze scale formation and deposition caused by water injection.
Evidence of the formation of CaSO4, SrSO4, and BaSO4

e
Yassin [72] precipitants.

Polson et al.
ESEM
P r
To measure the wettability of quartz surface with and without biofilms Identification of wettability alterations from hydrophilic
[92]

Blkoor and
(bacterial/ fungal colonizations).

a l towards hydrophobic condition.

Fattah [93],
Al‐Yaseri et
SEM-EDS
r n
To investigate the influence of XC-Polymer on drilling fluid filter cake
properties and formation damage.
SEM analysis provided a good method to study the structure,
morphology and average quantitative chemical compositions
al. [94]

o u of the filter cake.

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You et al. SEM-based determination of occurrence state and morphology of salts SEM images showed that chlorite and illite/montmorillonite
SEM
[95] within the pore spaces of tight sandstone sample. were the main clay minerals in the samples.
To investigate rheological properties and formation dynamic filtration The result of SEM indicates formation of nano-filter cake that
Zhang et al.
SEM damage evaluation of a novel nanoparticle-enhanced viscoelastic surfactant can decrease the amount of viscoelastic surfactant fracturing
[96]
fracturing system constructed with wormlike micelles. fluid filtration.
SEM imaging confirmed a preferential adsorption of NPs
Abhishek et To visualize the adsorption of silica nanoparticles on Berea sandstone and obtained by static adsorption tests and visually shows that
SEM
al. [97] their effect on fluid/rock interaction during LSW flooding. more NPs adhere/adsorb on quartz surface compared to
kaolinite while it did not lead to blockage of pore throats.

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Khan et al. To investigate the morphology of gel injection’s formation damage before SEM imaging is applicable to analyze the variation in viscosity
SEM
[98] and after treatment with ultrasonic waves and chemical agents. of gel sample and efficiency of ultrasonic waves stimulation.
Direct evidence of fines migration as a formation damage
Yang et al. To investigate formation damage due to fines migration induced by the mechanism using SEM imaging of core sample, SEM-EDS
SEM-EDS
[99] leak-off of low salinity potassium chloride (KCl) fracturing fluids. analysis of produced solids and close matching of lab data with
an analytical model.

Zhao et al.
[100]
SEM
To evaluate formation damage mechanisms associated with drilling and
completion fluids for deep-water reservoirs.
o f
The main mechanisms of formation damage by drilling and
completion fluids were analyzed based on pore throats
blocking by solid invasion in which are ideal for formation of

r o an external filter.

p
Azizi et al. To analyze the impacts of scale inhibitors on the morphology and SEM analysis revealed that scale inhibitors can affect the
SEM
[101] deformation of precipitated scales.

e - shape of scale crystals.

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SEM imaging suggests that, owing to the high heterogeneity of
Ghamartale
SEM To determine pore structure alterations after ultrasonic treatments. dolomite samples, ultrasonic wave treatments were not

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et al. [102]
effective.

You et al.
[103]
SEM-EDS

a l
To investigate fines migration in geothermal reservoirs.
Illite/chlorite and kaolinite deposition caused permeability
reduction in geothermal reservoirs.

Wang et al.
[104]
SEM-EDS

u rn
To detect fines migration throughout the hydrate dissociation processes.
Formation damage caused by fines migration was identified
using SEM imaging.

Abbasi et al.
[105]
SEM-EDS
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To determine the morphology and composition of mixed salt precipitation
that may occur during smart water injection in carbonate formations.
To analyze the effect of a capillary-entrapped phase on fines migration in
The results of SEM-EDS analysis suggest SrSO4 as the
dominant produced scale that affects mixing of the injected
water with formation water.
Presence of a residual phase significantly decreases the
Prempeh et
SEM-EDS engineered sand-packs with different percentage of kaolinite and residual magnitude of formation damage and the amount of produced
al. [106]
oil. kaolinite.
SEM-EDS analysis evidenced the migration of fine particles
Wang et al. To analyze reservoir damage during acidizing for high-temperature and
SEM-EDS and subsequent blockage of the pore throats with a consequent
[107] ultra-deep tight sandstone.
decrease of permeability.

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3.2.2. X-Ray Diffraction (XRD)

XRD is a powerful nondestructive method to analyze the structural parameters of crystalline
materials based on phase identification through comparison with a reference database of X-
ray diffraction patterns [108, 109].

Application of this technique in the oil industry dates several decades, including for the
analysis of rock composition, mineralogy and clay fraction identification [54, 110], studies of
the effect of temperature and pressure on clay swelling [111], and measuring the density of
grains [112]. It has been also used to study various types of formation damage, such as the
reduction of permeability due to clay swelling [113] and KCl brine injection [114].

In pioneering research, Gkay and Rex [115] employed a combined XRD and SEM technique
to analyze clay migration where they concluded that dispersion of kaolinite or mica needles

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was the root cause of formation damage in sandstone core samples.

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Zhou [116] discussed the application of XRD analysis to determine the effect of fluid and
overburden pressure, temperature, pH, salinity and brine composition on clay swelling in
aqueous solutions in which was later developed by Zhou et al. [111]. They also concluded
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that osmotic swelling can cause more severe formation damage in compared with crystalline
swelling.
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Krishna et al. [117] employed XRD analysis of clay samples to evaluate the dependency of
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basal spacing of smectite on the type of cations and suggested crystalline swelling as the
main cause for reduction in the recorded permeability values. Following from this work,
Amorim et al. [118] revealed a stronger control over clay swelling for CaCl2 brine samples
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compared to NaCl and KCl solutions based on the results of XRD analysis.

Al Moajil and Nasr-El-Din [119] analyzed the manganese citrate precipitated during
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acidizing operations using a combined XRD, XRF (X-ray fluorescence) and ESEM method
where they found a direct relationship between the magnitude of precipitation and initial
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concentration of acid and temperature. It was also recommended that high-pH fluids should
not be used for cleaning of wells drilled with Mn3O4-based fluids.

Combining SEM-EDS, X-Ray Diffraction (XRD) and Nuclear Magnetic Resonance (NMR)
analysis methods (which is described later), Zhou and Nasr-El-Din [120] investigated
interactions of phosphonic-based hydrofluoric acid with clay minerals in sandstone cores as a
function of initial acid concentration, reaction time, and temperature. At the end, no trace of
aluminum fluoride (AlF3) in the reaction products was identified through elemental analysis
of kaolinite, bentonite, and illite samples while the story was different for the case of chlorite
mineral. Figure 3 shows a comparison of the chlorite spectrum before and after treatment that
confirms the presence of F peak in the spectrum.

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Figure 3. (Top) Elemental analysis of chlorite before treatment with full-strength phosphonic-based HF
acid; (Bottom) Elemental analysis of chlorite after treatment with full-strength phosphonic-based HF acid
at 77ºF for 24 hours [120].

Recently, Ahmad [121] investigated the role of flow rate and fluid alkalinity on fine particle
movement using XRD diffractometric plots of selected sandstone core samples (examples are
shown in Figure 4). They suggested that migration of illite, kaolinite, chlorite, and fine
particles of other minerals is the main cause for reduction in permeability based on the results
of XRD and SEM analysis.

X-ray diffraction offers a technique complementary to direct imaging, allowing the chemical
composition of fines material and other causes of formation damage to be determined with
great accuracy. Usually these studies are performed in combination with imaging to allow
the structure and nature of the damage to be determined as well.

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Figure 4. Examples of XRD patterns of selected sandstone core samples [121].

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3.2.3. X-ray Computed Tomography (CT) scanning
X-ray imaging is an extremely powerful and nondestructive technique to probe the internal

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structure of rock samples [122, 123]. The first CT scanners were introduced by Hounsfield in
1969 and became commercially available in 1972 when this technology was employed in the
-p
UK for widespread medical use [124, 125].

In the petroleum industry, CT scanners were first used in the 1980’s [126, 127] to determine
re
reservoir rock characteristics [128]. As listed in Table 3, they can be categorized into four
classes based on object size and spatial resolution. The instruments can either be adapted
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medical scanners with limited power and resolution, industrial or special-purpose X-ray
instruments designed for high resolution, as well as imaging using bright synchrotron
radiation which allows images to be acquired in a few seconds [129].
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Table 3. A general classification of existing X-ray computed tomography based on Carlson et al. [130].
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Type Scale of observation Scale of resolution

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Conventional (medical) m mm

High-resolution industrial dm 100 µm

Ultra-high resolution industrial cm 10 µm

High-resolution micro-tomography mm µm

a) Formation damage analysis using conventional CT-scanning

Gilliland and Coles [131] used conventional CT-scanning (a low-power adapted medical
scanner) to investigate the severity and location of the damaged zones. In the same way,
Ozgen Karacan et al. [132] suggested that the CT-scan technique is a reliable method to
evaluate the homogeneity or heterogeneity of core samples.

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Bartko et al. [133] revealed the efficiency of CT-scanning to evaluate acidizing systems and
the associated reactions between acid with minerals. Vickerd et al. [134] also employed this
technique to investigate the influence of acid gas flooding on morphology, size, and
distribution of the pore structure, as well as fine dislodgement and desiccation.

Mahmoud [135] assessed the scale damage from precipitation of calcium sulfates during low
and high salinity water injections and, using CT imaging, observed a greater magnitude of
damage inside the core samples flooded with high salinity water.

Tran et al. [136] presented a good example from a combined CT scanning and Nuclear
Magnetic Resonance (NMR) to analyze the formation damage mechanisms for a single phase
flow core-flooding. NMR is described later in this paper.

Khan et al. [137] conducted a couple of experiments to analyze the particle flow infiltration

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while flooding into soda-lime glass bead core samples. Using modified medical CT-scanners,
they measured the variations in porosity caused by fines migration.

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In a recent study, Shamsi et al. [138] used CT-scanning to study the damage occurred by
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injection in both heterogeneous and homogenous porous media where they observed a non-
uniform damage pattern even in homogenous core samples. They also realized a greater
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magnitude of damage in the inlet of core samples.

The problem with the use of conventional X-ray imaging using adapted medical scanners is
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that they provide images of rather poor resolution and cannot accurately capture the texture of
the pore space and certainly cannot elucidate pore-scale mechanisms. Industrial scanners
have more power, but are more expensive, and are not routinely used in oilfield applications,
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despite having far superior imaging characteristics [139]. Furthermore, imaging has to be
combined with other techniques, such as XRD or XRF to provide chemical information
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[140]. What is needed is a non-destructive imaging technique with micron resolution,

described next.
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b) Formation damage analysis using micro-CT scanning

The recent advent of micro-CT imaging has provided new understanding of the pore-scale
structure of the rocks and the fines and fluids within them [54]. Moreover, a deeper insight
into the interactions between drilling/completion fluids and host rock can be achieved
through a combination of micro-CT scanning and other available imaging methods at
different scales [9, 67].

Applications of this method for the characterization of drilling-mud filter cake and damage
have been reported in several studies, such as, Elkatatny et al. [141] and Green et al. [54].
The latter presented a novel approach named ―difference mapping‖ that is based on a
combination of common geological methods and micro-CT scanning scanning to quantify the
change in rock structure due to damage.

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In a case study on an oil filed in East Malaysia, large field 3D micro-CT scanning
accompanied by Field Emission Scanning Electron Microscopy (FESEM), Pore Network
Modeling (PNM) methods and a set of petrophysical analyses were used to identify
homogeneous regions of core plugs and to exclude the damaged zones during coring
operations [142]. The authors suggested a combination of micro-CT and PNM as an
innovative option to quantify the potential influences of core-flooding experiments on
multiphase flow and to identify the sensitivities of core handling.

Later, Ma et al. [143] investigated the evolution and internal damage of hydrated shales based
on micro-CT scanning and found a gradual increase in damage variables against immersion
time with the highest rate of damage during the initial steps.

Using a combination of micro-CT and SEM-EDS, Yu et al. [144] found an 80% of reduction

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in permeability caused by clay migration during fresh water injection while a smaller 50%
decrease was estimated through image-based computations. Moreover, the observed increase

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in intensity of CT number near the core outlet was attributed to fines straining and clay
relocation. -p
Yang et al. [145] employed 3D micro-CT imaging to analyze the potential damage
mechanism of Dongying sandstone during workover fluid flooding and formation liquid
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flooding. Meanwhile, the changes of pore structure before and after displacement were
quantified based on micro-CT intensity profile, pore radius and coordination number that
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suggested the pore spaces were partially blocked by clay minerals and moving particles.
Figure 5 presents examples from segmented 2D slices and 3D visualizations of the sample.
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Figure 5. Raw (top) and segmented (middle) 2D slices and 3D segmented pore space (bottom) through
sample 2 (24 μm resolution, pore space is purple and rock matrix is dark blue); dry sample: (A1), (A2),
(A3); sample after workover fluid flooding: (B1), (B2), (B3); sample after formation liquid flooding: (C1),
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(C2), (C3) [145].

Table 4 summarizes the main formation damage studies based on CT and micro-CT scanning
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techniques, not including the work already discussed.

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Table 4. A list of previous work on CT & micro-CT applications in formation damage analysis (sorted in chronological order).

Author(s) Method Aim(s) Main achievement(s)

A compacted zone with variable thicknesses was
To analyze the porosity damage in crushed zone around the identified along the perforation tunnels during perforation
Karacan and
CT perforation tunnels caused by shaped-charge perforating of gas-saturated rock samples, though they could not
Halleck [146]
operations. observe any compacted zone in the case of liquid-
saturated samples.

Okwen [147] CT
To investigate asphaltene-based damage during tertiary CO2
flooding.

o f
Imaging showed that reducing the concentration of
formation water acting as a CO2 buffer in crude oil can
minimize the flocculation of asphaltenic components.

r o
To study the filtrate invasion in sandstone core samples during
More realistic in-situ monitoring of filtrate invasion of
oil-based drilling fluids was permitted using CT images

p
Guo et al. [148] CT
core-filtration analyses. accompanied with core-flooding experiments compared

e - with HPHT filter press tests.

Yerramilli
[149]
et al. CT
Optical petrography
To investigate
reinjection.
injectivity

P r
decline during produced-water Face plugging at injection face and surface deposition
caused injectivity declines in porous media.

Ma and Chen [150] micro-CT

a l
To characterize meso-damage in shale hydration.
Rapid growth of micro-cracks was found in early soaking
time, which is considered as the main meso-damage

r n period.

Hu et al. [151] micro-CT

o u
To study the mechanisms
interactions in shale reservoirs.
of proppant-fluid-formation
Treatment fluids can decrease the proppant embedment
effect and maintain the effective fracture width.
Moreover, proper selection of treatment fluid is crucial in

Grove et al. [127] micro-CT

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To investigate perforation damage.
reducing the formation-damage-related costs.
High quality quantitative data were achieved on porosity
and permeability in both native rock and around the
crushed zone.
To analyze the fracturing fluid saturation after leak-off and flow- Shut-in wells drilled in shale formations and tight
Ibrahim and Nasr-
CT back steps as well as the impacts of soaking time on regained sandstones caused significant decreases in regained flow
El-Din [152]
characteristics. rates and permeability.
Formation damage mechanisms can be efficiently
Godinho et al. To analyze the particle invasion, migration and deposition in
CT analyzed using quantitative time-lapse radiography which
[153] porous media based on time-lapse radiography.
can ease the optimization of drilling and EOR fluids.

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3.2.4. Nuclear Magnetic Resonance (NMR)

The NMR technique is another method used for the analysis of rock samples: the spins
contained principally in protons are aligned in a magnetic field; when the spins relax, the
resultant electromagnetic signal is detected [154]. NMR provides a fast, nondestructive, and
convenient tool for the characterization of complex porous media [155-157].
The measurement of how the NMR signal decays, and the total signal, can be used to infer
the pore size distribution, porosity and fluid distribution [53, 158]. Liu et al. [159] also used
NMR to quantify the motion of water within a core sample.
Tandon et al. [160] assessed the application of NMR to evaluate proppant packs and
associated mechanical damage. It was concluded that NMR analysis is quite sensitive to
permeability and pore structure, presence of fines, mechanical damage, and proppant coating
and type.

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Guo et al. [156] examined water sensitivity, solid phase adsorption, and damage caused by

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CarboxyMethyl Guar (CMG) and HydroxyPropyl Guar (HPG) gum fluids using a
combination of NMR-based experiments, mercury injection analysis, SEM, and core-
flooding tests. They could provide a micro-perspective basis for analysis of damage
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mechanism, type and origin.
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Recently, Wu et al. [161] developed a new experimental method to evaluate the formation
damage induced during drilling of sandstone reservoir based on a combination of NMR
analysis and large-sized model tests. It was found that reservoir permeability and overbalance
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pressure can affect both degree and depth of the damage while rate of permeability alteration
was found to be higher in low permeability sandstones.
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In addition, Lufeng et al. [162] employed a combination of NMR, SEM and Pressure
Transmission Tests (PTTs) to evaluate damage in sandstone formations. The results of NMR
analysis revealed that the internal reasons for water-blocking and water-sensitivity damage
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are related to the amounts of mobile water and bound water, respectively.
Bageri et al. [163] investigated secondary formation damage during the filter cake removal
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process using combined NMR, micro-CT and core flooding techniques. Figure 6 shows the
NMR analysis of the pore structure before and after injection of a barium-saturated chelating
agent that releases barite precipitates into the pore space and absorbs cations from either
minerals or other pores. Note that, in this study, micro-CT analysis rejected the idea that
wormholes were generated due to invasion of filter cake solvent and its subsequent
interaction with the rock matrix.

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Figure 6. (Top row) Incremental pore volume and cumulative porosity for sandstone sample obtained
from NMR measurements. (Bottom row) Incremental pore volume and cumulative porosity for a
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carbonate sample [163].

Kamal et al. [164] used a combination of NMR, SEM and core-flood experiments to study
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the effect of clay mineral concentration on formation damage during water/HCl injection in
sandstone formations and concluded that chlorite and illite clay minerals control pore throat
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plugging and permeability reduction.

In a recent study, Gomaa and Mahmoud [165] studied formation damage resulting from
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injection of traditional mud acids into illitic sandstones and introduced a novel method of
stimulation based on in situ generated Hydro-Fluoric (HF) acid. They used the results of
NMR analysis to demonstrate the generation of micro fractures and increase in porosity of
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the core samples due to mineral dissolution.

The key feature of much of this work is the use of a combination of methods to study
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formation damage. Table 5 lists other work where several different approaches have been
used to elucidate the damage mechanism and quantify its effect on pore structure and
productivity.

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Table 5. A brief summary on the combined application of formation damage analytical approaches.

Authors Methods Aim(s) Major achievement(s)

Experimental
approach including:
static and dynamic  Local saturations and pressure measurements are crucial for the
To explain the relationship between filtration rate and identification of the extent and amount of damage.
invasion tests, and
Longeron et permeability impairments. 

f
characterization of Polymeric non-salted mud induced a small damage on moderate
al. [166] To plot the porosity and oil & water saturation profiles.
both external and clayey sandstones containing viscous crude oil.
internal mud cakes
using Cryo-SEM

o o
To analyze the primary damage mechanism during water-

p
 r
-
The significance of damage during brine injection was observed
flooding in clay-rich reservoirs.
to be a strong function of mineralogy.

e
Leone and XRD, SEM and To evaluate the characteristics of permeability damage during


r
The occurrence of a critical velocity, along with other
Scott [25] TEM water injection.
observations, indicate that the primary damage mechanism is
To distinguish between likely damage mechanisms, such as,

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fines migration, and clay swelling and dispersion.
To investigate the permeability reduction in sand packs caused

fines migration.

a
Aliaga et al. Effluent concentrations, including the produced solids, can be
CT-scanning, SEM by solids generation and migration.
[167] simulated based on a fractional flow model for solids migration.

Rahman et
Thin-section, XRF,
XRD, SEM,
u rn
To study the effect of ion exchange and fluid flow on
formation damage of reservoirs containing illitic clay minerals.
 XRD study confirmed that illite present in the sandstone
samples is susceptible to swelling and migration.
al. [168] capillary pressure
and porosity tests

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Morphology of illite in pore spaces of this sandstone and its
influence on petrophysical properties.



Above a critical salt concentration, however, the illite remains
attached to the pore walls.
The study revealed loss of permeability and porosity due to
proppant dissolution and subsequent remineralization in the
Weaver et SEM-EDS, XRD, To study the damage caused by geochemical reactions between pack.
al. [169] and XRF proppant and formation.  Damage depends on the composition of both the proppant and
the formation materials that should be considered when
selecting a proppant for high-temperature or high-stress wells.
 Precipitation and deposition inside pore spaces were identified
SEM, XRD, X-ray
Mohsenzade To investigate the formation damage due to deep eutectic as the main sources of formation damage based on the results of
CT along with core
h et al. [170] solvent used as an EOR agent. SEM and quantitative XRD analysis.
flooding tests.
 CT-scanning was used to observe the damage.

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 It was revealed that barite particles were first trapped in thin

SEM, NMR, micro-
Al-Yaseri et Pore-scale analysis of formation damage in Bentheimer pore throats prior to filling the adjacent pore spaces.
CT and core-
al. [67] sandstone.  The volume of trapped fines decayed rapidly against the depth
flooding
of core sample.
 A greater magnitude of damage was observed in case the rock
SEM, NMR, micro-
Al‐Yaseri et To investigate the impact of fines and rock wettability on surface and the fine (Barite) particles had the same wettability.
CT and core-
al. [94] reservoir formation damage.  Wettability controls the 3D distribution of fines in the pore
flooding
space.



o f
The flow paths of chemical solutions and the location of well
affect the distribution of formation damage.

o
SEM, TSA, XRD, Absorption and scaling mainly lead to a decrease of
Li et al. To analyze the formation damage during alkaline-surfactant-

r
adsorption and ion permeability-porosity at injection and production wells
[171] polymer (ASP) flooding.
analyses. respectively.

- p
 Corrosion and grain migration mainly result in increase of
permeability and porosity at intermediate distances.

r e  The intensity of heat is determinant in changing the structure,

texture and mineralogy of sandstone.
Wang et al.
[172]
XRD, SEM, X-ray
CT and NMR
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To study the effect of microwave heating on petrophysical
properties of sandstone samples and to eliminate the formation
damage caused by water blocking and clay swelling.
 The growth of micro-fractures into larger fractures or pores, can
be reflected by the change of T 2 distribution of fully saturated

a
samples.
 Intergranular fractures were identified based on SEM imaging of

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treated samples.
 19
F NMR showed that AlF3 and in the spent acid were the
Ji et al.
[173]
NMR, SEM-EDS
and 19F NMR u
To better understand the mechanism of AlCl3 working as a

o
retarding agent in mud acid. 
only two aluminum fluoride complexes.
More can complex with Al in the Al-based retarded mud-

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acid system than in the mud acid system, which could lead to a
deeper penetration of the acid into the formation.
 Identification of the extent of potential permeability impairment
NMR T2 spectrum,
induced by alkali sensitivity.
MRI image and
 Chlorite and illite dispersion and migration were determined as
quantitative
the main triggers for damage.
Fang et al. evaluation of To investigate the alkali sensitivity damage mechanisms in
 Generation of silicide precipitation due to reactivity of rock
[174] minerals by tight oil reservoirs.
framework with hydroxide is another important alkali sensitivity
scanning electron
damage mechanism.
microscopy
(QEMSCAN)  Variations in pore distribution resulted from alkali sensitivity
damage can be observed through MRI analysis of the cores

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exposed to the fluids with high pH values.

 Shale pores were blocked by silica nanoparticles and the

AFM (atomic force To investigate the application of silica nanoparticles and average pore size was reduced by 50%. This phenomenon can
Yang et al.
microscopy) and environmentally-friendly materials (high-temperature mitigate pore pressure transmission, reduce the permeability by
[175]
SEM resistance mud) for shale gas horizontal drilling. 98%, and thus enhance the wellbore stability.

Assem et al. NMR, SEM-EDS,

To investigate the factors affecting the interactions of regular

o f
o
Cristobalite dissolved in the mud acid more than mullite, which
mud acid with sand and clay-based proppants under downhole

r
[176] XRF and XRD. can cause fines that might reduce proppant-pack conductivity.
conditions.

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 With the increasing thickener contents and filter loss of
fracturing fluid, core permeability regains turned to be declined.
Dai et al.
[177]
SEM, microscope
system, NMR
r
permeability alteration in tight oil reservoir cores.
e
To study the effect of supercritical CO2 fracturing fluid on  Tight cores were more likely to receive more damage in
permeability.

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
The retention of thickener in microchannels (micro pores) were
confirmed to be the main mechanism for permeability alteration.
Low-viscosity fluid was found to have more formation damage
Kamal et al. SEM, NMR, and

n a
To identify the effect of rheological behavior of viscoelastic

potential compared with the high-viscosity one.
NMR and core-flooding results revealed that the damage took
[178] core-flooding

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surfactants on formation damage in carbonate rocks.

u
place both in pore bodies and pore throats. However, most of the
surfactant was retained in pore throats.

Radwan et
al. [179]
TSA, SEM-EDS,
XRD
J o
To introduce a diagnosis work flow to find location and
potential source of damage, and recommend a suitable
treatment method.



The proposed formation damage diagnosis work flow was
effective and can be applied at any oil or gas well.
Geological studies, petrographic description and mineral
identification are very important tools in evaluation of formation
damage.
Low-temperature  Lignite reservoirs with different pH have different degrees of
Wang et al. ash (LTA)+XRD To study water and salt sensitivities in lignite reservoir under water-sensitive damage. Partial alkalinity and acidity conditions
[180] combined with different pH. are strongly water sensitive, while strong alkalinity conditions
(SEM) are weakly water sensitive.
Mahmoud
To study the effect of flooding sandstone core samples with  Optimal EDTA solution concentration was determined so that
and Al- XRD, SEM, CT
high pH EDTA chelating agent solutions and subsequent oil there was no fines migration, clay swelling, and non-clay
Hashim scan, and NMR
recovery process. minerals dissolution.
[181]
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 Gray Bandera core samples were found to exhibit

incompatibility with a solution of more than 5 wt% of EDTA
and the high permeability enhancement because of the
interaction of EDTA with ankerite mineral.
To investigate the adsorption and retention of hydroxypropyl  The adsorption and retention of guar gum in tight gas reservoirs
Li et al. SEM, AFM, NMR guar gum (HPG) fracturing fluid in porous medium as an resulted in a decrease of the pore to throat size ratio, and the
[182] and CT-scanning important factor affecting the production in tight gas most adsorption occurs at grain edges and rock beddings.
reservoirs.

Hajiabadi et CT-scanning and

To investigate rheological and formation damage behaviors of
invert oil emulsions (W/O) with the addition of the carbon-


o f
Results proved the dazzling performance of smart nanomaterial
in diminishing the severity of pore plugging.

o
al. [183] SEM
based nanomaterials.  Nanomaterial additives are highly efficient.
Micro-CT, Itrax-

p

r Mineral dissolution (dolomite and other high-density minerals)

-
XRF scanning,
Othman et To investigate the mechanism of fines migration during CO2 dislodged quartz and clay mineral fines.
SEM-EDS and

e 
al. [184] injection. The permeability damage can be explained by fines migration
nitrogen
permeability

P r 
and subsequent blockage.
Results showed that severe fluid sensitivity damage occurred

l
with a decrease in fluid salinity, and an increase in pH values.


a
Abnormal low water saturation, mixed wettability, abundant
SEM, XRD,
Zhang et al. To understand the mechanism of formation damage during clay minerals, and complex pore structures are contributing to

rn
mercury intrusion
[185] drilling process in the ultra-deep fractured tight gas reservoirs. the severe phase trapping damage.
tests and etc.
 As a result of a smaller particle size distribution compared with

o u 
the larger natural fractures, the existing drilling fluids show a
high dynamic damage rate and poor loading capacity.

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The pore sizes affected the damage mechanisms and suffered
SEM, NMR and from obvious reduction as a result of water-sensitivity damage.
Zhang et al. To investigate mechanisms of formation damage from water
pressure- In fact, small pores were damaged by swelling of mixed-layer
[186] and alkali sensitivity for a reservoir in China.
transmission tests illite/smectite, and the large pores suffered from the combined
damage of swelling of smectite and migration of illite.
SEM-EDS, XRD
and X-ray To investigate water/rock interactions during hydraulic  It was suggested that the reuse of non-treated flow back water in
Zhang et al.
Photoelectron fracturing in Marcellus shale and to evaluate the formation field hydraulic fracturing operation can cause blockage of larger
[187]
Spectroscopy damage caused by reinjection of flow back water. pores and flow pathways.
(XPS)

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 CT-scanning and SEM revealed the significant effect of NPs in

drilling fluids on reducing the depth of penetration.
Hajiabadi et CT-scanning, SEM To study the effect of surface modified nano-silica on drilling
 There was less signs of drilling fluids component in the outlet
al. [188] and core-flooding fluid and formation damage.
face of the cores injected by drilling fluids containing surface
modified with NPs.
 Extended interaction of mud filtrate with Buff Berea sandstone
rock can cause severe formation damage as mud particles, clay
swelling, and fines migrations plug pores and throats of the

f
To evaluate the effect of exposure time on unconfined
rock.
Gamal et al. NMR and SEM- compressive strength and the integrity of pore system of Buff


o
NMR results confirmed that there was a corresponding increase
[189] EDS Berea sandstone rock samples due to the interaction with
in formation damage as shown by a progressive decrease in the
barite-weighted mud.

r o
rock porosity and permeability with time.
The exposure time was found to be a controlling factor for both

- p

reducing the rock unconfined compressive strength and porosity.
The dominant formation damage mechanism for sandstone rock

r e with calcite cementing material found to be associated with

silica dissolution/precipitation effects.
Kudrashou
and Nasr-El-
Din [190]
CT-scanning, XRD
and SEM-EDS
P
To investigate the formation damage associated with mineral

l
alteration and formation of swelling clays caused by steam
injection in sand packs.
 For sand packs with quartz, kaolinite, and carbonate minerals
this mechanism was shown to be associated with kaolinite-fines
migration.

n a  In mixtures of quartz with montmorillonite formation damage

was mainly caused by clay swelling, which led to filling of

u r
To investigate lost circulation material (LCM) soaking process

pores with montmorillonite.

o
Yang and SEM and micro-CT images indicated that a longer soaking time
SEM, micro-CT on fracture plugging for fluid loss remediation and formation
Chen [191] could lead to a less porous and strengthened plug structure.

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damage control.
To visualize the invasion depth of drilling mud particles and to  The effectiveness of bridging agents depends both the size of
Ismail et al. SEM and core evaluate the effect of bridging agent (calcium carbonate) particles and the concentration of the bridging agent.
[192] flooding tests particle size and distribution on permeability and porosity near  The size calcium carbonate should be almost identical to the
wellbore. pore throat median size of the formation face.

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3.3. Other analytical approaches to study formation damage

There are other – more advanced and experimental methods – to study formation damage.
These techniques may become more widely adopted as the technology develops.

3.3.1. Magnetic Resonance Imaging (MRI)

In this technique, imaging is based on NMR response as a function of spatial position of the
protons [174] that is accepted as a non-destructive and robust technique for visualization of
formation damage [138].

Baldwin et al. [193] reported the efficiency of MRI to detect and quantify the formation of
hydrate and dissociation in sandstone samples. In another research, Ersland et al. [194]
revealed the efficiency of a combined MRI and Nuclear Tracer Imaging (NTI) for the

of
evaluation of selected EOR methods in fractured oil reservoirs. They also demonstrated that
MRI is useful to study multiphase flow behavior in fractured porous media.

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Krebs et al. [139] presented the application of a combined MRI and micro-CT scanning
method for visualizing of the wormholes induced during acid stimulation of selected
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carbonate samples.
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Afrough et al. [195] used MRI to analyze fines migration inside core samples undergoing
water-shock fines-migration experiment, and to map the T2 distributions. They observed
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opposite trends in T2 spectra of the core inlet and outlet where their pore-size distribution
were shifted to larger and smaller values, respectively. This suggests the average pore size
increased at the inlet of the core and reduced at the outlet, consistent with sweeping fines
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through the core where some fines were retained near the outlet. The authors stated that
permeability impairment can be demonstrated using MRI and be applied to remedial or
preventive processes during fines migration.
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Further, Brattekås et al. [196] used MRI method to find the relationship between
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petrophysical parameters of oil-saturated fractured carbonate samples and leak off rate of
hydrolyzed polyacrylamide (HPAM) gels. The results verified the presence of a stabilized
displacement front as well as presence of wormholes in the gel.

Li et al. [197] employed a combined MRI, QEMSCAN and numerical simulation method to
analyze the extent of porosity and permeability damage, and evolution of mineral content in
tight reservoirs during water-flooding process. The study introduced clay migration and
swelling as the main causes of water sensitivity in ultra-low permeable reservoirs.

3.3.2. Focused Ion Beam and Scanning Electron Microscopy (FIB-SEM)

This technique produces high-resolution 3D image using a combination of high resolution

SEM and the precise milling capability of FIB which permits destructive access to the inner
structure of a sample [198]. While the resolution of the images is unparalleled, the method

27
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requires a long time of operation, only studies a small eroded area with a small observation
range, and has a high cost in terms of equipment and expert operation [199].

Note that the development of FIB technique dates back to the mid-1970s at the University of
Chicago and it improves the imaging resolution through prevention of hardness-related
surface topographic variations [200]. The main principle of the apparatus is similar to SEM
instruments, except that in FIB-SEM systems an ion beam is rasterized over the sample
sequentially as the FIB cuts through the material. Secondary electrons generated via the
interaction between sample surface and ion beam can then provide high-spatial-resolution
images. Moreover, the Ga ions used in the majority of commercial FIB-SEM systems enable
a precise machining of the sample [201].

It has been shown that FIB-SEM can provide microstructure analysis obtaining

of
unprecedented 3D resolution of a few nm. This method has been applied to image both
unconventional shale samples as well as sandstones [202, 203]. Further work is needed to use

ro
this method to look at formation damage specifically. Here the challenge is to image a
representative region of the pore space where sample preparation and imaging has not itself
damaged the structure.
-p
Lubelli et al. [204] used cryo-FIB–SEM technique to determine the effect of drying on clay
re
minerals and concluded that drying can significantly change the total porosity and pore size
distribution in bentonite while the impacts are milder in the case of kaolinite. In a similar
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study, Bai et al. [205] visualized different type and abundance of nano-pores between 5 and
100 nm, reconstructed the 3D pore structure, and calculated tortuosity, permeability and
porosity.
na

Arciniegas and Babadagli [74] analyzed precipitation of asphaltenes in heavy oils where the
morphology of organic deposition on the surface of glass beads was characterized using FIB-
ur

SEM. The results revealed a systematic increase in the thickness of asphaltene and showed
the significance for calculation of organic deposition surface roughness using FIB-SEM in
Jo

the characterization of formation damage at different operational conditions.

3.3.3. Acoustic tomography (AT) technique

Acoustic attributes of rock samples can be determined using Acoustic Tomography (AT)
which can be used to construct acoustic velocity tomograms to quantify damage caused by
deformation phenomena, such as pore collapse, dilatant and elastic deformations, and normal
consolidation phenomena [3].

Yamamoto [206] reconstructed high-resolution images of compressional wave velocity from

various bottom sediments based on high-frequency cross-well acoustic tomography. A 3D
wave-number spectra of the velocity variabilities along with the transformation procedures
from velocity image to the images of porosity, density, shear strength, and permeability were
determined for each measured velocity image.

28
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Scott et al. [207] conducted two distinct type of experiments including recording the
acoustic-wave velocity of samples during rock mechanical tests, and acoustic imaging of
deformation using compressional-wave velocities to construct tomographic images from the
localized pore collapse damage formed in a confined-indentation test. It was concluded that
the extension of such technology is beneficial to monitor the production and mechanical
reservoir damage.

Li et al. [208] employed acoustic tomography of unconsolidated porous rocks with residual
paraffin saturation and found that acoustic attenuation is sensitive to the microscale- and
grain-scale distribution of residual saturation (i.e. residual saturation strengthens the grain
contacts).

Based on a couple of rock mechanics tests including velocity measurements of S and P

of
waves, Soares and Ferreira [209] proposed a new method to analyze the mechanical
formation damage caused by drilling and production operation. They showed that this

ro
approach allows an accurate evaluation of near-wellbore analysis.

Barri et al. [210] used a combined acoustic and CT-scanning approach to analyze the impact
-p
of wormholes on elastic properties in carbonate rocks treated by ethylenediaminetetraacetic
acid (EDTA) and diethylenetriaminepentaacetic acid (DTPA) chelating agents. The results
re
were indicative of the fact that stimulating with chelating agents had no special effect on
mechanical attributes of harder samples, such as Indiana limestone cores, while significant
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changes were observed in the case of the weaker ones, such as Austin chalk.
na
ur
Jo

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3.4. Benefits and drawbacks

Table 6 presents a brief comparison of the existing methods based on their main advantages and disadvantages. In summary, imaging methods
provide valuable information that cannot be obtained by conventional methods. In combination, modern methods of imaging and analysis can
elucidate formation damage mechanisms and quantify their effects.

Table 6. A brief comparison of the main damage analysis approaches with their pros and cons.

Method Main applications Benefits

o f Drawbacks

o
 Time consuming
Darcy’s law  Estimation of relative and absolute permeability
and fluid saturation
 Non-destructive

p r
 Convenient and simple method
 Cannot be used in a range of conditions
including unsteady-state unsaturated and

e - saturated flow, flow in fractured rocks and

granular media.

Optical petrography
 Description of texture, fabric and sorting of rock
samples
 Identification of primary and secondary porosity
P r
 Convenient and simple method
 Destructive
 Analysis of fracture, relative abundance of
minerals and cement/matrix
a l  Time-consuming

r n  Expensive
 Difficult sample preparation
Transmission
Electron Microscopy
o u
 Analysis of the inner structure, morphology,  It provides high-quality and
 Sensitive to vibration and external magnetic
fields
(TEM)
J
composition and crystallography of a sample detailed images.  Samples are limited to those that are electron
transparent, able to tolerate the vacuum
chamber and small enough to fit in the
chamber.
 Images are in black and white
 High resolution topographical  Expensive instrumentation
imaging  Potential artifacts from sample preparation
Scanning Electron  Analysis of the size, shape, composition,
 Elemental analysis  Sample preparation may distort material
Microscopy(SEM) crystallography, and other physical and chemical
 Rapid  Sensitive to vibration and external magnetic
properties of a specimen
 Allows the examination of fields
samples such as metals, alloys and  Images are in black and white
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ceramics, as well as polymers and  SEMs are limited to solid, inorganic samples
biological materials small enough to fit inside the vacuum
chamber that can handle moderate vacuum
pressure.
 Non-conductive samples must be coated with
an additional thin layer (sputter coating)
 Non-destructive
 Only identifies crystalline solids
 Rapid
 Identification of the content and type of minerals  It is not able to locate each mineral in space
X-Ray
Diffraction (XRD)
 Can provide information on the structural
parameters of crystalline materials, such as phases,



Inexpensive
Convenient and simple method

o f  X-Rays do not interact very strongly with

light elements

o
Interpretation of the resulting data
texture (preferred crystal orientations), average  Relatively low sensitivity

r
is relatively straightforward
grain size, strain, crystal defects, and crystallinity.  Preparation of samples may require grinding
 It requires preparation of a


- p
minimal sample for analysis
High image quality and spatial
them down to a powder

CT-scanning and
 Imaging, quantifying properties and determining 
r e
resolution
Non-destructive
 Expensive
 Limited information on chemical element

P
Micro-CT distribution
the distribution of fluids in porous rocks  Rapid
 Monochromatic until color coded by operator

a l 


Provide 2D and 3D images
Provide accurate measurements
Non-destructive
 Rendering of the images is time-consuming

rn
Nuclear
 Rapid
Magnetic Resonance  Transport processes, petrophysical phenomena,  Low sensitivity
 Easy sample preparation
(NMR)

o u
and chemical reactions in porous media
 Can be used as a portable
instrument
 Expensive

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4. Conclusions
This study presented an overview of formation damage, which is one of the most challenging
problems that occur during the production of oil and gas reservoirs. The different types of
analytical techniques used to describe and understand formation damage have been described
briefly and then assessed with illustrations of example applications in the literature. The
emphasis of this review has been on image-based methods, summarizing the main
applications, advantages and drawbacks of traditional methods, electron microscopy, X-ray
Diffraction (XRD), Computed Tomography scanning (CT-scanning) and Micro-CT imaging,
and Nuclear Magnetic Resonance (NMR).
While numerous efforts have been made on the development of novel approaches for
formation damage analysis, more research is still needed to allow a routine comprehensive
analysis. Specifically we recommend that the techniques described in this paper are used in

of
combination – no single method provides a full assessment of the nature of the formation
damage while quantifying its effects on pore structure and productivity. Instead an integrated

ro
approach is required which combines traditional methods, such as permeability measurement
and optical microscopy, with more recent developments in high-resolution non-destructive
-p
3D imaging.

Conflict of Interest
re

The authors declare that they have no conflicts of interest.

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Highlights

 Imaging and analytical approaches have greatly improved formation damage studies
 Combined imaging and traditional techniques provide a powerful analysis approach
 Non-destructive imaging combined with NMR and SEM promise further
improvements

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Declaration of interests

☒ The authors declare that they have no known competing financial interests or personal
relationships that could have appeared to influence the work reported in this paper.

☐The authors declare the following financial interests/personal relationships which may be
considered as potential competing interests:

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