Deep Underground Science and Engineering - 2023 - Vandeginste - Mineralogy Microstructures and Geomechanics of Rock Salt

Received: 23 December 2022 | Revised: 15 February 2023 | Accepted: 13 March 2023
DOI: 10.1002/dug2.12039
INVITED ARTICLE
Mineralogy, microstructures and geomechanics of rock salt

for underground gas storage
Veerle Vandeginste1 | Yukun Ji2 | Frank Buysschaert3 | George Anoyatis4
1
Department of Materials Engineering, Abstract
Division Surface and Interface Engineering
Materials, KU Leuven, Campus Bruges, Rock salt has excellent properties for its use as underground leak‐proof
Bruges, Belgium containers for the storage of renewable energy. Salt solution mining has long
2
State Key Laboratory for Geomechanics and been used for salt mining, and can now be employed in the construction of
Deep Underground Engineering, China underground salt caverns for the storage of hydrogen gas. This paper presents a
University of Mining and Technology, Xuzhou,
wide range of methods to study the mineralogy, geochemistry, microstructure and
China
3
geomechanical characteristics of rock salt, which are important in the engineering
Department of Mechanical Engineering,
Division Applied Mechanics and Energy
of safe underground storage rock salt caverns. The mineralogical composition of
Conversion, KU Leuven, Campus Bruges, rock salt varies and is linked to its depositional environment and diagenetic
Bruges, Belgium alterations. The microstructure in rock salt is related to cataclastic deformation,
4
Department of Civil Engineering, Hydraulics diffusive mass transfer and intracrystalline plastic deformation, which can then be
and Geotechnics Section, KU Leuven, Campus associated with the macrostructural geomechanical behavior. Compared to other
Bruges, Bruges, Belgium
types of rock, rock salt exhibits creep at lower temperatures. This behavior can be
Correspondence
divided into three phases based on the changes in strain with time. However, at
Veerle Vandeginste, Department of Materials very low effective confining pressure and high deviatoric stress, rock salt can
Engineering, Division Surface and Interface exhibit dilatant behavior, where brittle deformation could compromise the safety
Engineering Materials, KU Leuven, Campus of underground gas storage in rock salt caverns. The proposed review presents
Bruges, Bruges, Belgium.
Email: veerle.vandeginste@kuleuven.be the impact of purity, geochemistry and water content of rock salt on its
Yukun Ji, State Key Laboratory for
geomechanical behavior, and thus, on the safety of the caverns.
Geomechanics and Deep Underground
Engineering, China University of Mining and KEYWORDS
Technology, Xuzhou, China.
creep, hydrogen, impurities, rock salt, salt solution mining, underground gas storage
Email: jykcumt@163.com
Funding information Highlights

Onderzoeksraad, KU Leuven,
Grant/Award Number: STG/20/013
• Hydrogen may become indispensable in the transition to renewable energy
• Rock salt caverns may provide leak‐proof containers for hydrogen storage
• Mineralogical composition links with depositional environment and diagenesis
• Microstructure links to cataclastic deformation, diffussive mass transfer and
intracrystalline plastic deformation
• Geomechanical behavior of rock salt is influenced by its composition and
impurities
1 | INTRODUCTION are commonly mined and used in many industrial

applications. Rock salt is extracted either by rock mining
As a sedimentary type of rock, rock salt is formed by or by solution mining. The latter method pumps fluids
chemical precipitation from a saturated fluid that has into underground to dissolve the salt, and then pumps
undergone solar evaporation. This generally occurs in the resulting brine back up to the surface; in this way, the
arid climate systems, in Salinas, perennial lakes and salt is then recovered, and underground rock salt caverns
sabkha environments. Upon primary precipitation, the are formed accordingly.
salt sediments commonly undergo diagenetic processes, Recently, rock salt caverns received more attention
resulting in secondary rock salt textures. Rock salt has for their potential use as underground energy storage
been mined for a very long time, with records dating (hydrogen, natural gas, compressed air) or disposal of
back to 4700 years ago. Halite, anhydrite and gypsum waste (radioactive waste). In particular, the European
This is an open access article under the terms of the Creative Commons Attribution License, which permits use, distribution and reproduction in any medium, provided
the original work is properly cited.
© 2023 The Authors. Deep Underground Science and Engineering published by John Wiley & Sons Australia, Ltd. on behalf of China University of Mining and
Technology.
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130 | VANDEGINSTE ET AL.
target of net zero greenhouse gas emissions by 2050 This review places its focus on the characterization of
involves a policy towards hydrogen supported electrifica- the mineralogy, geochemistry and microstructures in salt
tion. Because of the limited energy density of batteries rocks and their impact on the macrostructural deforma-
(Yazawa & Shakouri, 2021), the use of hydrogen may tion properties. Rock salt composition can vary widely,
become indispensable, in particular for long haul from almost pure halite to mixed compositions. A recent
transportation, such as trucks, buses (Li, Djilali, study indicates that the use of nonrepresentative rock salt
et al., 2022), or aircraft (Verstraete, 2015), which can samples due to heterogeneity, and thus differences in the
rely on fuel cells or internal combustion engines to type of quantity of impurities, can result in poor rock salt
convert chemical power to useful power. Also, the characterization and lead to optimistic design criteria
incentive of governments to emit less greenhouse gases (Azabou et al., 2022). Moreover, the structure of rock
and become less dependent on fossil fuels for grid salt varies with domal salt and bedded salt deposits.
electricity generation, contributes to a substantial growth Several key challenges in the field remain unresolved.
in wind and solar energy production (Androniceanu & How does microstructural deformation translate to rock
Sabie, 2022). Unfortunately, the amount of energy salt's macroscale geomechanical properties? How can
produced by these systems relies strongly upon favorable upscaling be addressed from microscale models to field
meteorological and seasonal conditions, and the energy scale salt cavern predictions? How does rock salt
availability is therefore not necessarily in tune with the composition (salt impurities and second phase content)
power demand (Zhang, Liu, et al., 2022). This causes influence its geomechanical behavior? How does the rock
systems to be used below their capabilities or not at all salt setting (domal salt, diapir, bedded salt) affect its
(Zhang, Liu, et al., 2022). A solution to recover this lost geomechanical properties? To what extent is humidity
potential is to convert the excess available power into and water content in rock salt samples impacted through
hydrogen by electrolysis and store it in rock salt caverns removal from their burial environment by drilling or
(Murray et al., 2018). This technique has the potential to mining, and what are the implications for geochemical
cover the seasonal energy deficits observed during winter and geomechanical changes in the samples?
time. Caverns should be considered as part of a larger
hydrogen distribution network and could provide the
necessary energy buffering and thus stability in the 2 | MINERALOGY AND
energy provision (Ozarslan, 2012), either by delivering GEOCHEMISTRY OF ROCK SALT
hydrogen directly to the end user, such as trucks and
aircraft, or by converting it back into electricity by fuel 2.1 | Rock salt and depositional environment
cells or gas turbines to support the grid. The durability
and reliability of hydrogen storage is important and it is Rock salt is a rock that is mainly composed of salt,
therefore essential to perform profound studies on the generally halite (NaCl). This term is used in mining,
storage of hydrogen in rock salt caverns. engineering and industry settings, whereas evaporite is
Rock salt has excellent properties for providing a commonly used in geological (sedimentologic, diage-
leak‐proof container due to its porosity of less than 0.5%, netic) context. The major rock salt deposits consist of
permeability of less than 10−21 to 10−20 m2 (Bérest halite (NaCl), anhydrite (CaSO4), and gypsum
et al., 2001), its plastic behavior (creep), self‐healing (CaSO4 · 2H2O), but also other minerals such as sylvite
properties and high thermal conductivity. The sealing (KCl), polyhalite (K2Ca2Mg(SO4)4 · 2H2O), carnallite
properties of rock salt have been proven through (MgCl2 · KCl · 6H2O). Halite and sylvite are colorless in
geological time by trapping oil and gas. Hence, under- their pure form, but they can show a color due to the
ground rock salt caverns are considered to be a presence of trapped air bubbles, fluid inclusions, finely
potentially suitable solution for underground storage of dispersed clay (Figure 1), organic matter, hematite, KBr,
renewable energy. This is critical to meet energy demand and lattice defects (Sonnenfeld, 1995). The clay present in
fluctuations effectively when the electricity grid supply is rock salt has a detrital origin, and is commonly illite,
deficient. The safety of storage in the underground kaolinite, chlorite, smectite or mixed‐layer clay
reservoirs is crucial both in the short and long terms.
Despite the excellent sealing capacity, salts may locally
leak, introducing major hazards. In particular, rock salt
permeability can drastically increase by several orders of
magnitude for a dilatancy increase of only 0.1% to 0.2%
(Schulze et al., 2001). An excellent review on the
potential leakage of salt with implications for mine and
cavern stability on short and long term is presented by
Warren (2017). Several other research papers have been
published on rock salt properties, followed by a few
examples. A comprehensive overview of microstructures
in rock salt can be found in Urai et al. (2008). The
mechanical behavior of salt and salt caverns is discussed
in Berest (2013). Peach and Spiers (1996) described the F I G U R E 1 Wall and roof in the Winsford underground salt mine
influence of microplastic deformation on permeability (United Kingdom) with thinly bedded halite with varying degrees of
using synthetic salt rock. impurities consisting of mainly clay, some quartz and anhydrite.
DEEP UNDERGROUND SCIENCE AND ENGINEERING | 131
(Warren, 2006). The variation in salt mineralogy is linked

to its depositional setting and diagenetic environment.
Due to chemical precipitation, rock salt forms a
saturated saline solution at the surface, generally in
saline lakes in arid or semi‐arid environments. The
composition of rock salt is thus related to the deposi-
tional setting and the hydrochemical nature of the parent
brines (Osichkina, 2006). The texture of the rock salt,
however, is generally secondary due to diagenetic
processes in shallow burial or postuplift settings, rather
than primarily associated with the depositional setting,
since rock salt dissolves easily (Warren, 2006).
Evaporation of seawater and other saline fluids will
lead to the precipitation of certain salts in a specific order F I G U R E 2 Chemical evolution of brine from evaporation of
based on the composition of the parent fluid and current seawater. Plot of ionic concentration versus degree of
environment. For the evaporation of current seawater, evaporation, based on data from McCaffrey et al. (1987).
it is determined that salt precipitation proceeds in the
following order: aragonite (at twice the concentration of
seawater), gypsum (at 4–5 times the concentration
of seawater), halite (at 10–12 times the concentration of
seawater), and then potassium or magnesium sulfates
and chlorides (predominantly carnallite and epsomite),
when supersaline fluids reach concentrations of 70–90
times that of seawater (Carpenter, 1978; McCaffrey
et al., 1987) (Figure 2). Geological rock salt layers may
present a different order since the composition of
seawater has changed through time (Warren, 2006).
Rock salt is not only formed through evaporation of
seawater, but in saline lakes with a different mineral
assemblage, such as sodium carbonate minerals (trona,
nahcolite, shortite), sodium silicate minerals (magadiite
F I G U R E 3 Powder X‐ray diffraction scan of rock salt samples
and kenyaite) and sodium or calcium borate minerals
from Winsford Mine (United Kingdom) with mainly halite, and minor
(Smoot & Lowenstein, 1991). Saline lacustrine deposits anhydrite and quartz.
are commonly classified based on salinity, or they can be
distinguished as carbonate or sulfate types with certain
composition and distribution of salt and clay minerals crystals (Figure 3). The diffractograms are analyzed and
(Qi et al., 2021). Besides evaporation, additional quantified using PXRD software with reference data-
processes can lead to the formation of rock salt, namely bases of ICCP PDF series and Rietveld analysis. The
temperature changes (Sloss, 1969), mixing of brines PXRD method cannot be used for the detection of very
(Raup, 1982), and brine freezing (Sonnenfeld, 1984). small amounts or trace contents of certain minerals in
samples, since those signals may not be distinguishable
from the background noise or from the diffraction peaks
2.2 | Methods of mineralogical identification of the major constituents.
The preparation of samples for PXRD analysis varies
The most common method for mineralogical identifica- and depends on the amount of available material, bulk
tion of rock samples is powder X‐ray diffraction (PXRD) analysis versus analysis on separated fractions, and
analysis. The principle behind the PXRD method is the randomly oriented versus oriented mounts. Common
Bragg's equation, which presents the relation between the PXRD analysis is performed on randomly oriented bulk
angle at which constructive interference occurs (θ) sample, which is prepared by crushing the rock sample to
between waves of wavelength (λ) and the distance powder, and placing it in a holder for PXRD measure-
between atoms on lattice planes in a crystal (d ): ment. Because of the small size of clay particles, the
signal from the clay in samples can be fairly weak in
2d sin θ = nλ. (1) nonoriented bulk samples. Therefore, additional sample
preparation is carried out to separate the clay fraction
Angles of constructive interference are measured by from the bulk sample, using ultrasonication of the
an electronic detector that records the intensity of the sample in an aqueous solution with sodium hexameta-
signal while the sample is scanned over a range of phosphate to disperse the particles, and centrifugation to
diffraction angles. The PXRD method is used to identify separate the heavier particles of the sample from the
the mineralogical assemblage of samples, as it provides supernatant with clay. Oriented clay mounts are then
information on the crystal structure of the sample prepared by gravitational settling of the clay from the
constituents based on the diffraction pattern that is clay suspension on the mounts. Analysis of the clay
characteristic for the position and type of atoms in mounts by PXRD provide clear reflections, and further
differentiation between clay minerals is facilitated by on their affinity to bind with a positively charged
additional chemical treatments in terms of swelling of stationary ion exchanger by Coulombic interactions.
clays or dissolution in hydrochloric acid or by heat The concentration of anions in fluid samples is deter-
treatments (Moore & Reynolds, 1997). mined through comparison of signals with calibration
Another conventional method of mineralogical iden- fluids of a series of concentrations.
tification of rock samples is petrographic analysis using Geochemical elemental analysis can also be con-
an optical polarizing light microscope. Such analysis is ducted on the (powdered) rock sample, without the need
conducted on 30 µm thin slices of rock by passing light for dissolution, by X‐ray fluorescence (XRF) spectrome-
through the sample. Different minerals interact differ- try (Hancerliogullari & Eyuboglu, 2020; Quye‐Sawyer
ently with light due to their different internal structure et al., 2015). In this case, the sample can either be a
and composition, and this enables identification of the polished surface of a rock sample, powdered rock
minerals. Using this petrographic method with magnifi- sample, or a pressed pellet made from powdered rock.
cation, not only major constituents but also minor or XRF is a nondestructive technique, whereby a sample is
trace minerals in the sample can be identified, as well as irradiated by high energy X‐rays that cause excitation
the rock texture. and ejection of electrons from an inner orbital shell of
Automated mineral identification systems linked to atoms in the sample. As a consequence, an electron from
scanning electron microscopes include the Mineral a higher orbital shell will fall down to fill the created
Liberation Analyser (Ferrari et al., 2021; Ji et al., 2021) vacancy in the lower shell, and with this, a fluorescent
and QEMSCAN instruments (Ma et al., 2016; Zhao, X‐ray is emitted. The emitted radiation is characteristic
Zhang, et al., 2022). The method is based on high‐ for the transition between shells of specific elements,
resolution backscatter electron image analysis, energy which enables identification of elements in the sample,
dispersive X‐ray analysis and automated microscope and the intensities of the radiation allow quantification
operation and data acquisition, and is usually employed of the concentrations of these elements.
on thin sections or polished thick sections. The technique Geochemical elemental analysis of polished sections
involves automated collection of mineralogical maps of or thin sections can be performed by electron probe
samples. Moreover, it can generate large, statistically microanalyzer (EPMA). EPMA works in a similar way
representative datasets of porosity, grain size and shape, to a scanning electron microscope. The sample is
mineralogical associations and digital textural maps. A bombarded with an electron beam, which results in the
disadvantage of the technique is that polymorphs, such emission of X‐rays at wavelengths that are characteristic
as calcite, aragonite and vaterite, cannot be distin- for specific chemical elements. This method allows for
guished, and it is also difficult to distinguish between high resolution analysis and automated geochemical
minerals with very similar chemical compositions, such mapping of samples. In contrast to the above methods,
as gypsum and anhydrite. Differentiation of polymorphs EPMA enables very detailed small‐scale analysis rather
and minerals with similar composition can be easily than bulk analysis of samples (Vandeginste et al., 2020).
made using PXRD, as discussed above. For example, geochemical zoning of minerals can be
documented and mapped at micrometer scale by EPMA.
Geochemical isotopic methods such as sulfur, oxy-
2.3 | Methods of geochemical gen, chlorine and bromine isotopes have been applied to
characterization evaporites (Ding et al., 2019). These isotopic analyses are
used to identify the source of the brine that has formed
Geochemical characterization of rock salt can be related the rock salt and to distinguish between marine and
to the mineralogical composition, and it provides nonmarine origin. Fluid inclusions in salt crystals can
additional information on impurities within phases, and provide more information on the formation temperature
data which can help identify the origin of the brine that and geochemistry of the brines (Wang et al., 2016),
precipitated the salt. similar to how information is derived from fluid
Powdered rock samples can be dissolved using inclusions in other minerals (Vandeginste et al., 2017).
aqueous (acidic) solutions, and then the concentrations Besides the general geochemical characterization of
of the cations in the solutions are measured by rock salt, it is also important to determine the water
inductively coupled plasma optical emission spectrome- content, in particular in studies that involve geomecha-
try (ICP‐OES) or mass spectrometry (ICP‐MS). An nical rock salt analyses. Water is present in rock salt
inductively coupled plasma is generated by ionization of samples as interstitial brine, in hydrated minerals and as
argon gas in an intense electromagnetic field, resulting in fluid inclusions within crystals (Jockwer, 1982; Roedder
excited atoms and ions that emit radiation of character- & Bassett, 1981). In situ, resistivity analysis can be used
istic wavelengths. The intensity of the emissions at to predict water content in rock salt. In small rock salt
specific wavelengths is related to the concentration of samples, thermogravimetric analysis (TGA) is employed
specific elements, and these can be quantified by using a to determine and quantify the types of water in the
calibration series. With OES, concentrations can be samples (De Las Cuevas & Pueyo, 1995). The TGA
measured down to parts per million, whereas MS can be measurement records the changes in the mass of the
employed to measure concentrations down to parts per sample while the temperature increases over time. In
trillion. Measurements of anions in the fluids are addition, Fourier transform infrared (FTIR) spectrome-
conducted using ion chromatography. With anion‐ try has been used to measure water content in rock salt
exchange chromatography, anions are separated based samples, and a calibration for this was established with
synthetic samples (Ter Heege et al., 2005). Using this stress to the uniaxial compressive strength (Zhang,
technique, high spectral resolution data are generated for Wang, et al., 2022). Moreover, the tests show that the
the infrared spectrum of adsorption or emission of a number of large pores and total pores increase and the
sample. The wavenumber of 1650 cm−1 corresponds to number of small pores decrease after 12 000 cycles
the bending vibration of the water molecule in a (Zhang, Wang, et al., 2022).
saturated NaCl solution. Second, diffusive mass transfer is a deformation
mechanism that, at temperatures of up to about 200°C in
the diagenetic domain, proceeds via solution and
3 | M IC R O S T R U C T U R E S precipitation, resulting in textures with corroded grain
OF ROCK SALT surfaces and overgrowths. The mechanism involves
material removal in the direction of maximum pressure
3.1 | Deformation microstructures leading to fabrics with indented, truncated and inter-
and mechanisms penetrating grain boundaries, and material addition in
the direction of minimum pressure resulting in textures
Three deformation mechanisms and corresponding with overgrowths (Blenkinsop, 2002). Thus, grains
microstructures (Figure 4) can be distinguished: (1) dissolve at highly stressed contact points and form a
cataclastic deformation with the development of micro- brine fluid film, and this material diffuses towards the
fractures and rotation of displacement of grains without zones of lower stress, where the material then precipitates
permanent lattice distortion, (2) diffusive mass transfer (Schutjens & Spiers, 1999). This dissolution, diffusion
with removal, transport and deposition of material with transport, and precipitation is driven by the difference in
permanent lattice distortion or melting, and (3) intra- chemical potential between the highly stressed contact
crystalline plastic deformation with permanent lattice grain boundaries and the intergranular zone under lower
distortion without fracturing (Blenkinsop, 2002). One of stress. Diffusive mass transfer can also result in fluid
the characteristic features of rock salt is its plastic inclusion planes that are perpendicular to the direction of
deformation behavior that occurs already at relatively minimal stress. Moreover, studies have shown that
low temperature and low confining pressure in compari- diffusion can occur at much lower temperatures and
son to that for other types of rocks (Urai & Spiers, 2007). lower differential stress in wet rock salt than in dry rock
First, the cataclastic deformation mechanism involves salt (Urai et al., 1986). Diffusive mass transfer micro-
microcracking or frictional sliding. Microcracks are structures are distinguished from cataclastic microstruc-
called intragranular when they occur within single grains, tures due to the lack of microfractures. And they are
transgranular when they cut through multiple grains, or different from intracrystalline plastic deformation micro-
circumgranular when they occur at grain boundaries structures, for they do not have undulatory extinction,
(Blenkinsop, 2002). Brittle deformation with microcrack subgrains or recrystallized grains in their fabrics. As
development, grain rotation and dilational behavior previous studies have shown, the diffusive mass transfer
occurs in rock salt only at very low effective confining process can be linked to the intergranular plastic
pressure and high deviatoric stresses (Cristescu & deformation process (Urai & Spiers, 2007). Pressure
Hunsche, 1998; Peach & Spiers, 1996; Peach et al., 2001). solution creep is driven by diffusive mass transfer that
This dilation domain is separated from the compaction occurs at the grain boundaries, it facilitates intracrystal-
domain with ductile, creep deformation by the dilatancy line plastic deformation in the form of dislocation creep,
boundary (Cristescu & Hunsche, 1998; Van Sambeek and this process is very rapid in halite (Schenk et al., 2006;
et al., 1993). Microfracture development in the dilation Urai & Spiers, 2007; Urai et al., 1987). Diagenetic halite
domain results in an increase in permeability in rock salt generally has a mosaic texture whereby crystal bounda-
(Van Sambeek et al., 1993). Deformation induced by ries meet at triple junctions of nearly 120°, which might
microcracking at low effective mean stress can thus lead be facilitated by a pressure solution mechanism
to the formation of percolating pore space, commonly (Warren, 2006). Diffusive mass transfer can also occur
observed in the zone of disturbed rock around openings at higher temperatures in the metamorphic domain, and
in salt mines of nuclear waste repositories, and in high then it occurs in the solid state. There are two main types
overpressure underground environments (Ghanbarzadeh of solid state diffusive mass transfer. Nabarro–Herring
et al., 2015). Cyclic loading tests on rock salt have creep is caused by volume diffusion movement of lattice
indicated that the number of developed intergranular defects in the crystal lattice, and Cobble creep is the
cracks increases with the ratio of maximum cycling result of solid state diffusive mass transfer through grain
F I G U R E 4 Schematic presentation of deformation microstructures in rock salt. (a) Rock salt crystals before deformation. (b) Cataclastic
deformation microstructures. (c) Diffusive mass transfer microstructures. (d) Intracrystalline plastic deformation microstructures.
boundaries triggered by chemical potential gradients acoustic emission method, and porosity distribution
linked to internal strain energy gradients. using nuclear magnetic resonance technique. Several
Third, intracrystalline plastic behavior involves the types of sample preparation are applied to enhance
movement of dislocations, and also solid state diffusion microstructure visualization, and multiple types of
in some mechanisms. A dislocation is a defect or microscopy are used such as polarization microscopy
imperfection in the crystal lattice, and the movement with transmitted light and incident light and scanning
of dislocations happens by breaking bonds in the electron microscopy. Rock salt samples are particularly
original lattice ahead of the dislocation and reforming challenging in terms of preparation of thin sections for
the bonds behind the dislocation. There are two main microscopic study, mainly because of the solubility of
types of dislocation movement: dislocation glide by salt in water, the impact of humidity, and the effect of
movement along slip planes, and dislocation climb by water content in the samples on microstructures and
the change of slip plane of edge dislocations. Disloca- geomechanical properties. Therefore, rock slabs of salt
tion creep involves deformation by both dislocation samples need particular preparation by either dry sawing
movement types. Even at low confining pressures of or preparation using oil.
10 MPa, dislocation creep is important in rock salt in Transmitted light microscopic analysis is conducted
the diagenetic domain (Urai & Spiers, 2007). Disloca- on thin sections and enables observation of fluid
tion creep causes several phenomena, namely (i) inclusions that are aligned at high angle grain bounda-
undulatory extinction due to the crystal lattice distor- ries. The inclusions can have various shapes, such as
tion, (ii) the formation of subgrains that have a slightly arrays of isolated bubbles, elongated bubbles or tubes, or
different crystallographic orientation than the rest of even almost continuous films. Some sample treatment
the grain, and (iii) the formation of new grains during techniques have been documented that can further help
dynamic recrystallization by subgrain rotation and microstructure identification. First, observation of grain
grain boundary migration. Subgrain boundaries are and subgrain boundaries is facilitated by chemical
oriented approximately perpendicular to the dislocation polishing and etching of mechanically polished samples
glide direction, and the subgrain diameter correlates in 5.5 M NaCl solution with 0.8 wt% FeCl3 · 6H2O for
with deviatoric stress (Carter et al., 1993). Intracrystal- 10 s, followed by rinsing the surface with n‐hexane and
line plastic deformation causes flattened or elongated drying with hot air (Urai et al., 1987). Incident light
grains with a preferred orientation, and the movement microscopy was used to study the etched salt sample
of dislocation causes strain ellipsoids. Grain shape surfaces. Such microscopic analysis enables distinction
fabrics can also result from the coalescence of grains between high angle grain boundaries and subgrain
with similar orientation during dynamic recrystallization, boundaries by deeply etched and less deeply etched lines,
with grain boundary migration driven by the internal respectively. Second, using the same etching solution but
strain energy gradient from a less‐deformed grain with leaving it dry slowly on an etched sample surface to
lower dislocation density to a more highly strained one enable NaCl epitaxial overgrowth provides information
(Ter Heege et al., 2005). High strain deformation on crystallographic orientation of salt grains (Friedman
experiments on relatively dry coarse‐grained rock salt et al., 1984). Third, additional microstructural informa-
show that dislocation creep is the main microstructural tion can be obtained through irradiation of salt samples
deformation mechanism without extensive dynamic with gamma radiation with dose rates of 20 to
recrystallization (Linckens et al., 2016). Fluid‐assisted 80 MRad/h for a total dose of around 5 × 109 Rad, and
grain boundary migration involves solution‐ at a temperature of 120°C (Urai et al., 1985). Such
precipitation transfer across grain boundary brine irradiation causes a blue coloration of the samples due to
films, driven by differences in chemical potential induced lattice defects, which enables visualization of
between grain boundaries linked to dislocation density microstructural features (Levy et al., 1981).
differences between old deformed grains and newly A scanning electron microscope (SEM) is used to
growing grains (Peach et al., 2001; Schenk et al., 2005, visualize microstructures and their morphologies
2006). Fluid inclusions at the grain boundaries (Martin‐Clave et al., 2021). Cryogenic scanning electron
are transformed into a grain boundary fluid film microscopy (cryo‐SEM) and environmental scanning
during both static and dynamic recrystallization electron microscopy (ESEM) allow the investigation of
(Ghanbarzadeh et al., 2015). The relative importance liquid or wet samples. This can be achieved by
of deformation mechanisms, such as dislocation creep investigation of the sample in the frozen state in the
and pressure solution, depends on temperature, con- case of cryo‐SEM whereby small rock samples are
fining pressure, grain size, solid solution impurities, subjected to shock freezing to approximately −190°C,
second phase content, and water content. or under reduced pressure in the case of ESEM.
Specifically, ESEM is employed for the study of rock
salt grain boundary healing. The use of ESEM enables
3.2 | Methods of microstructure the observation of water trapped at the surface of
identification particles and meniscus formation between adjacent
particles (Hwang et al., 1993). Cryo‐SEM has also been
Microscopy is commonly used to document microstruc- used to study fluid‐filled and healed grain boundaries by
tures, and more advanced techniques are used for three‐ observation of the boundary fluids in the frozen state
dimensional imaging of samples using X‐ray computed (Schenk et al., 2006). Similarly, the brine in grain
tomography, microstructural damage evolution using boundaries is investigated using broad ion beam
Acoustic emission (AE) is a common method applied

to the studies on the evolution of damage and crack
formation in rock samples. This method can be used for
real‐time monitoring, and can then be combined with
post‐test CT scanning of the rock sample. The AE
technique is based on sound waves that are generated
when microcracks are formed or are propagating
(Zhao, Ma, et al., 2022). This is a result of the release
of stored energy that builds up in the sample with stress
concentrations at certain locations (especially near pores
or already existing microcracks), due to external loads
applied on the sample during mechanical testing.
Analysis of the acoustic emission parameters including
F I G U R E 5 EBSD colored map indicating crystal orientation in
rock salt, adapted from (a) K. Liang et al. (2021), and (b) Desbois
events, energy and frequency‐amplitude distribution,
et al. (2010). allow for the reconstruction of the evolution of damage
in time and space in the rock sample. Research on rock
salt has demonstrated that the AE method can be used
cryo‐SEM to gain insights in the mechanism of static on plastic natural materials to investigate deformation
recrystallization of wet halite with the evolution of the under thermobaric conditions, and to study the effect of
grain boundary structure (Desbois et al., 2012). With this temperature and strain rate on fracture dynamics.
method, the broad ion beam is used to produce a cross Moreover, anomalous changes in AE activity allow the
section in the sample for further SEM investigation. distinction between the different stages of rock salt
Electron backscatter diffraction (EBSD) analysis deformation (Shkuratnik et al., 2020a). The AE method
(Figure 5) is used to determine the crystallographic has also been used to investigate the stress memory effect
orientation of grain boundaries in rock salt samples in uniaxial cyclic loading of rock salt samples under
(Schenk et al., 2006). For this type of analysis, the variable temperatures (Shkuratnik et al., 2020b). Addi-
samples need to be very finely mechanically polished tional work explored experimentally the rock salt
down to 4000‐grade carborandum paper polishing, dilatancy boundary using AE and triaxial compression
and 10 s chemical polishing with methanol, followed tests were carried out on rock salt samples from the Asse
by diethyl ether rinsing (Schenk et al., 2006). Before Salt Mine, Germany (Alkan et al., 2007). It is shown that
EBSD analysis, the samples were coated with carbon the AE could be used to determine the dilatancy
to reduce charging. Analysis of EBSD patterns boundary during the triaxial tests. AE test systems can
can be done using software through comparison with be further used to conduct experiments on bedded rock
calculated halite patterns, and EBSD maps are salt samples under uniaxial compression and indirect
further processed to remove erroneous data (Schenk tension. The failure state of bedded rock salt can be
et al., 2006). predicted by inspecting the variation between the stress
X‐ray computed tomography (CT) is a non- or the energy release, and the fractal dimension of the AE
destructive test employed for three‐dimensional visual- spatial distribution (Xie et al., 2011).
ization of microcracks in rocks by analysis of differences The nuclear magnetic resonance technique has been
in density (Zhao, Ma, et al., 2022). Different minerals used on rock salt to investigate pore characteristics of
can be distinguished in the rock samples (especially for healed rock salt samples after damage caused by uniaxial
minerals with significant differences in density), and compression (Chen, Peng, et al., 2020), and to study
digital processing of the CT images enables quantifica- changes in pore structure in rock salt subjected to cyclic
tion of pore and fracture space and different minerals. loading (Wang, Zhang, et al., 2022). Nuclear magnetic
The CT images are segmented and brightness is adapted resonance is the physical response of a nucleus that sits in
to enhance the contrast and improve the separation of a strong constant magnetic field and gets subjected to a
different regions (rock matrix vs. pore space, and weak oscillating magnetic field. Longitudinal and trans-
between different minerals). For example, anhydrite verse relaxation times are defined as the mean time for
impurities, pore space, and fluid phases along grain the magnetic moment of the nucleus to get back to its
boundaries, or intracrystalline fluid inclusions can be original state upon disabling the oscillating magnetic
visualized and quantified using micro‐CT (Thiemeyer field. Studies have derived a relationship between the
et al., 2015). A CT scan of the rock salt sample before transverse relaxation time T2 and the pore radius of a
geomechanical testing serves as a control to ensure rock (Ge et al., 2014). NMR technology has also been
sample integrity (Zhao, Ma, et al., 2022). Micro‐CT is employed to investigate water migration and gas
also used to identify the changes in the internal desorption in pore‐fracture systems using transverse
microstructures upon mechanical loading the rock salt relaxation time T2 (Zhang et al., 2019).
sample (Zhang, Agostini, et al., 2021). Moreover, the The pore structure of rock salt has also been
effect of the evolution of texture and internal stresses on studied using mercury injection porosimetry and gas
the relationship between permeability and applied stress adsorption testing (Chen et al., 2018; De Las Cue-
was studied by 3D synchrotron micro‐CT and 3D X‐ray vas, 1997). The method of mercury injection is based
diffraction on polycrystalline rock salt samples (Moslehy on mercury, a nonwetting fluid, entering pores in
et al., 2021). samples when the pressure exceeds the capillary
pressure. A pressure‐volume curve is generated by greater thermal expansion and insufficient porosity to
gradually increasing the applied pressure. The pore size accommodate the expansion. For example, at a temper-
can be correlated to applied pressure using the Washburn ature of 150°C and a depth of 5 km, halite shows an
equation. At very high pressure, the mercury injection expansion of 2% caused by heat and contraction of 0.5%
method could lead to some damage in the sample. due to pressure (Talbot & Jackson, 1987). Moreover, in
Therefore, another method, namely gas adsorption, is comparison to other subsurface sedimentary rocks that
used in particular for determination of small pores of less lose porosity and increase in density with deeper burial,
than 100 nm in diameter (Zhang, Wei, Vandeginste, halite becomes less dense than surrounding rocks from
et al., 2020). This method is based on adsorption isotherms about 1 km depth, which drives positive buoyancy of
using an inert gas, generally nitrogen. The pore size is rock salt. An overview of the density and Mohs hardness
correlated to partial pressure. Several adsorption theories of some of the most common minerals in rock salt
and models have been proposed for adsorption of differing (Giambastiani, 2020) is presented in Table 1. All minerals
gases in pores in various rock types, for example, CO2 in in rock salt are quite light, with the lightest being
shale (Xie et al., 2022). carnallite and sylvite, whereas anhydrite and polyhalite
are the heaviest. Gypsum and sylvite are the softest from
the series, and polyhalite and anhydrite the hardest.
4 | GEOMECHANICAL The geomechanical properties based on short‐term
CHARACTERISTICS OF mechanical tests are presented in Table 2. This overview
ROCK SALT is based on the studies and references compiled by
Giambastiani (2020). Anhydrite is not only the hardest in
4.1 | Rock salt physical and geomechanical the series of common rock salt minerals, anhydrite rocks
properties are also significantly stronger than gypsum rocks and
halite rocks (Bell, 1981). The average E‐modulus of
With low density that is, less than 2.3 g/cm3, low anhydrite rocks is also twice as high as that of halite
hardness that is, less than 3 on Mohs hardness scale, rocks and gypsum rocks (Table 2). Moreover, the
high solubility, low strength, rock salt typically deforms common rock salt types all show plastic deformation
easily showing creep behavior (Giambastiani, 2020). It before failure, and anhydrite rocks show the least and
has a higher thermal conductivity (up to 6 W/m K) than halite rocks the most amongst a comparison between
other rocks such as sandstone, mudstone or coal (Mello halite, anhydrite, gypsum, and sylvite rocks (Bell, 1981).
et al., 1995; Zhuo et al., 2016). The viscosity (as The rheological behavior of rock salt depends on
measured by the ratio of shear stress to the shear strain external factors, such as applied loading, confining
rate) of rock salt is also lower than that of other rocks, pressure, and temperature, as well as intrinsic properties,
and depends on the temperature and moisture content of including mineralogical composition, water content,
the rock (Warren, 2017). Rock salt has low porosity and texture, grain size, and impurities. Two deformation
permeability, and good self‐healing properties, making it domains, namely a dilatancy domain and a compaction
an desirable medium for underground gas storage (Liu & domain, have been established for rock salt (Cristescu &
Xiao, 2014). Halite has a density of 2.17 g/cm3 at room Hunsche, 1998; Van Sambeek et al., 1993); these are
temperature, which decreases with greater depth due to separated by the dilatancy boundary (Figure 6). The
latter depends on pore pressure and stress loading rates
(Alkan et al., 2007). Dilation is faster with higher pore
TABLE 1 Density and Mohs hardness of common rock salt pressure, and the dilatancy boundary values decrease
minerals. slightly with faster stress loading (Alkan et al., 2007).
Mineral Density (g/cm3) Mohs hardness Dilation, which is caused by microfracturing, results in
an increase in rock salt permeability (Van Sambeek
Halite 2.04–2.17 2.5
et al., 1993). This brittle deformation occurs at very low
Gypsum 2.20–2.40 1.5–2.0 effective confining pressure and high deviatoric stress
Anhydrite 2.20–2.98 3.0–3.5 (Cristescu & Hunsche, 1998; Urai et al., 2008), and leads
to damage of the rock structure. Dilation is higher with a
Carnallite 1.57–1.61 2.5 higher axial pressure, and faster dilation occurs for
Sylvite 1.86–1.99 2.0 slower unloading and at higher temperature (Zhao
et al., 2019). Dilatation or volume growth is of particular
Polyhalite 2.78–2.79 2.5–3.0
concern for the application of underground storage of
T A B L E 2 Strength (Brazilian test and uniaxial compressive strength), Young's modulus, Poisson ratio, cohesion, and friction angle for several
rock salt types.
Rock type Braz (MPa) UCS (MPa) E (GPa) ν c (MPa) ϕ (°)
Halite rocks 2.2 ± 2.2 28.5 ± 8.9 23.9 ± 12.6 0.31 ± 0.05 5.4 ± 2.9 38 ± 7
Anhydrite rocks 5.4 ± 1.7 75.7 ± 26.7 50.9 ± 25.1 0.30 ± 0.04 22.6 ± 16.2 34 ± 4
Gypsum rocks 2.5 ± 1.1 27.8 ± 10.2 23.1 ± 13.6 0.27 ± 0.06 10.8 ± 2.0 24 ± 2
expressed as the sum of the strain rate caused by

dislocation creep, and that caused by pressure solution
creep, which are functions of the respective activation
energy, temperature, and differential stress:
−Qd −Qp σ
ε̇ = Ae RT σ n + B e RT , (2)
TD m
where A and B denote constants related to deformation

rate (s−1); Qd is the activation energy for dislocation
creep (J/mol); Qp is the activation energy for pressure
solution creep (J/mol); R is the universal gas constant
F I G U R E 6 Dilatancy boundary between the compaction and (J/mol K); T is the temperature (K); σ is the differential
dilatancy domains for rock salt is presented as octahedral shear stress stress (MPa); D is the grain size; n is the exponential
versus normal stress, based on Schulze et al. (2001). factor for stress and m is the exponential factor for grain
size (Urai & Spiers, 2007). The correlations reflect that
dislocation creep is strongly dependent on differential
stress and pressure solution creep is heavily dependent on
grain size. Moreover, the creep behavior of interbedded
argillaceous rock salt is different from that of high purity
rock salt (Gao et al., 2022).
Creep has not only been studied under single‐stage
loading, but also with multistage loading. Results have
indicated that the crack development is more extensive in
samples that have experienced multistage loading in
comparison with single‐stage loading, and this damage
accumulation leads to deterioration of the rock salt
geomechanical properties (Dong et al., 2022). The effect
F I G U R E 7 Schematic evolution of strain versus time for creep
deformation of rock salt with indication of the three creep stages that of this damage accumulation is mainly reflected in the
may occur for a long‐term compression test with constant load and at transient strain and the strain in the transient creep
constant temperature. domain, whereas the steady‐state creep is related to stress
and temperature but independent of loading history
(Dong et al., 2022). The long‐term strength of rock salt
gas or hazardous waste. In the compaction domain, was determined and a nonlinear creep damage constitu-
deformation occurs in a ductile manner without the tive model was established by Wu et al. (2020) based on
formation of cracks or failures, and with salt deforma- multistage creep tests.
tion by creep due to movement of dislocations and elastic
deformation (Hunsche & Hampel, 1999). Such creep
deformation is time‐dependent. It is a very important 4.2 | Geomechanical testing methods
phenomenon in rock salt, where low stress results in large
strain without brittle failure. Macroscopic geomechani- Rock salt geomechanical testing can be conducted
cal behavior can be linked to microstructural mecha- using short term or long term experiments, uniaxial or
nisms. During dislocation creep, subgrains are formed, triaxial compression testing, and with static loading
and fluid assisted grain boundary migration may occur if or cyclic loading. The uniaxial compression test uses
water is present in the form of brine inclusions or compression along the length axis of the sample
grain boundary films (Schenk et al., 2005). Solution‐ whereas the sample is unconfined in the transversal
precipitation creep may take place alongside inter- direction. Under triaxial compression testing, com-
granular sliding and rotation. pression loads are applied both in the longitudinal
The creep behavior of rock salt can be split into three direction and in the transversal direction. Generally,
domains based on the change in strain with time, namely, cylindrical rock salt samples with a diameter of at
primary or transient creep, secondary or steady state least 10 times the crystal size, and a length‐to‐
creep and tertiary or accelerated creep (Figure 7). During diameter ratio of two (Hawkins, 1998), are placed
primary creep, the strain increases very rapidly at the between two steel platens and a layer of heat resistant
beginning, and then stabilizes gradually, leading to silicon tape. In particular for the triaxial experiments,
secondary creep where the strain rate is constant. the rock salt samples are also covered by heat shrink
Tertiary creep is the final stage of deformation before PTFE membrane to separate the sample from the
failure, when the strain rate increases exponentially until confining fluid (Martin‐Clave et al., 2021). Axial
failure. Also, under combined creep and fatigue, the extensometers and circumferential chain extens-
strain‐time curves show a similar pattern with the three ometers are attached to the sample to measure
domains of transient, steady state and tertiary creep dimension changes, and thus to derive strain and
(Ma, Wang, Wang, et al., 2021). The steady state strain Poisson ratio. The force transducer (load cell) enables
rate ε̇ (considering nondilatant deformation) can be measurement of the load applied to the sample.
Geomechanical tests can apply static loads, meaning cumulative cyclic damage in rock salt (Ma, Wang, Wang,
a constant load in the longitudinal direction, and in the et al., 2021). The study suggested that the life of the rock
case of triaxial loading also a load in the transversal salt can be predicted through the linear correlation
direction, for the entire duration of the experiment. By between the logarithm of the deformation rate in the
calculating the stresses and strains based on the steady‐state phase and the logarithm of the creep or
measurements during the experiment, the elasticity fatigue life, that is independent of the loading history
modulus and Poisson ratio can be derived. Triaxial (Ma, Wang, Wang, et al., 2021).
compression tests have also been combined with acoustic
emission measurements (Figure 8) to determine the
dilatancy boundary under a specific stress, stress loading 5 | IMPACT OF GEOCHEMICAL
rate and pore pressure (Alkan et al., 2007). Cyclic AND MICROSTRUCTURAL
loading is applied to test the fatigue strength and CHARACTERISTICS ON
behavior of the material (Wang, Zhang, et al., 2022). G E O MECH AN I CAL PRO PE RT IE S
In cyclic loading geomechanical tests, the cycling rate
and the number of cycles can be set. In general, cyclic The onset of dilatation is a criterion for the long‐term
loading of a material would be performed until failure to stability of the rock (Wang et al., 2015). Various
determine the fatigue strength at a certain maximum dilation criteria have been suggested. Hunsche and
stress and amplitude. Hampel (1999) suggested that the dilatancy boundary
Besides short‐term geomechanical tests that are used for rock salt is practically solely dependent on the stress
to determine rock salt properties, creep tests are condition and not on salt type, stress geometry, or
conducted, as time‐dependent or long‐term geomechani- loading rate. However, previous research has shown
cal behavior is very important for rock salt (Eslami that anisotropy, derived from bedded salt layers, should
Andargoli et al., 2019). The strength of rock salt is also be considered in the mechanical evaluation of rock
dependent on the strain rate. Rock salt can fail in a salt behavior (Hatzor & Heyman, 1997). As inelastic
brittle manner through the formation of fractures under deformation develops and volume growth under com-
high strain rates, but subsurface rock salt tends to flow pression follows, anisotropy influences both the stresses
(Talbot & Jackson, 1987). Creep tests apply static and rates of deformation. An empirical model for the
loading and are conducted over longer periods of time, compression‐dilation boundary in anisotropic rock salt
varying from at least several months to years (Lyu was presented by Hatzor and Heyman (1997) with the
et al., 2021). Very slow creep tests (with stages of 8 determination of the major principal stress at the onset
months) have been conducted on natural salt samples of dilation as a function of confining pressure and
under a small deviatoric stress range to assess the discontinuity orientation for the Mount Sedom salt
applicability of constitutive laws that are extrapolated rock samples. As these data show, stress at the onset of
from relatively high stress tests (Bérest et al., 2019). The dilation decreases with decreasing confining pressure
results showed that transient creep takes long (6 to 10 and with increasing angle of discontinuity orientation.
months) and steady‐state strain rates are much faster (7 to Later, new dilatation criteria were suggested by for
8 orders of magnitude faster) for these tests with small example, DeVries (2006) and Schulze (2007) and
deviatoric stress in comparison to that predicted by most successfully applied to the design of salt caverns. On‐
constitutive laws (Bérest et al., 2019). Furthermore, time‐ going efforts focus on improving models with dilatancy
dependent behavior has also been assessed using cyclic (Gunther & Salzer, 2012; Hampel, 2012), the efficiency
loading tests, whereby the effect of loading frequency was of healing in dilated rock salt with respect to humidity
evaluated and led to establishing a variable‐parameter and pore pressure (Popp et al., 2012), and prediction of
creep damage model (Ma, Wang, Wang, et al., 2021). post‐yield strength and deformation characteristics of
Another study using a similar method indicated a positive rock salt using a dilation angle model (Chen et al., 2016;
interaction between the time‐dependent damage and the Ma, Wang, Wang, et al., 2021). Moreover, triaxial
F I G U R E 8 Rock salt samples and triaxial deformation testing equipment with acoustic emission monitoring (Rock Mechanics and Physics
Laboratory, British Geological Survey, UK).
compression tests have been simulated in models using 12.8 MPa for the bedded salt and 11.1 MPa for rock salt
halite matrix with insoluble material impurities, and with distributed impurities. The presence of insoluble
show that the impurities can induce dilatancy with the material in rock salt also has a significant impact on
formation of microcracks (Azabou et al., 2021). creep behavior at elevated temperatures, which may be
Creep has the strongest impact on the time‐dependent linked to differences in thermal expansion (Tijani
strain and stress evolution in a system. Transient creep et al., 2012). Solid solution impurities and second phase
phases are history dependent, whereas the constant final content, as well as temperature, confining pressure, grain
steady state creep rate is considered to be only dependent size and the presence of water along grain boundaries
on stress and temperature (Hunsche & Hampel, 1999). strongly influence the type of microstructural deforma-
Steady state creep rate above the dilatancy boundary is tion processes and stress‐strain behavior that are at play
also dependent on humidity (Hampel, 2012; Hunsche & in rock salt (Urai et al., 2008). Under deformation at low
Hampel, 1999; Van Sambeek, 2012). The constitutive law deviatoric stress, impurities can cause anisotropic viscos-
of steady‐state mechanical behavior of rock salt is of the ity (Adamuszek et al., 2021). Furthermore, the mineral-
power law form, whereby the overall strain rate the sum ogical composition and texture of the rock influence the
is of an elastic and a viscoplastic component (Wang water content. The halite texture is related to brine in
et al., 2015). However, transient creep also needs to be the fluid inclusions, and the content of clay and sulfate
considered after a stress increase or decrease minerals have an impact on the intergranular brine
(Munson, 1997). Different types of rock salt exhibit (De Las Cuevas & Pueyo, 1995).
rather different creep behavior, which can originate from Anisotropy in rock sequences is an important factor
different distribution of microscopic impurities within (Tsang et al., 2005). Mudstone interbeds strongly impact
the grains (Hunsche & Hampel, 1999). The latter authors the rock salt strength and deformation properties.
developed a composite model based on experimental Uniaxial and triaxial compression tests on bedded
data, physical fundamental material behavior, and composite samples of anhydrite‐halite and mudstone‐
microstructural and macroscopic analysis. In this model, halite showed that the weakest component controlled
distribution of microscopic impurities and their effect on the overall geomechanical behavior (Liang et al., 2007).
creep can be taken into account by adapting the spacing Triaxial tests on the anhydrite‐halite composite samples
value in their model. Common impurities in rock salt show strain hardening with increasing confining pressure,
include mudstone, anhydrite, carnallite and sylvite, and and a trend towards halite‐dominated ductile behavior
they can occur as interlayers, laminae or aggregates (Liang et al., 2007). Studies have shown that uniaxial
dispersed within or at the boundaries of halite grains. compressive strength and elastic modulus correlate
The impurities in rock salt, their composition, and fabric negatively with the interbed thickness, and with the
contribute to the high variability in the mechanical distance between interbeds, but uniaxial compressive
properties (Cyran, 2021), as shown in Figure 9, The strength correlates positively with the number of interbeds
images on the left are the undeformed rock salt sample (Jiang et al., 2012). Swelling of marl interbeds under the
and those on the right are the rock salt samples after effect of water can impact convergence movement in salt
uniaxial compression test. The measured uniaxial com- mines (Hadj‐Hassen et al., 2012). Other studies have
pressive strength and Young's modulus were a bit larger shown that the strength of bedded salt rock correlates
in the salt with distribution impurities in comparison to positively with the strength of the soft interbed (Liang
the bedded rock salt. The dilatancy threshold was et al., 2012). Experiments with single layer anhydrite in
halite matrix demonstrate brittle behavior of anhydrite,
whereas halite behaves in a viscous way, resulting in tiny
prismatic anhydrite inclusions disseminated in a halite
matrix (Zulauf et al., 2009). Geomechanical tests on mixed
anhydrite‐halite rocks show that strength correlates with
anhydrite content (Price, 1982). A study on the Ocnele
Mari salt mine in Romania revealed that impurities in
rock salt could significantly change the viscosity of the
rock salt at low deviatoric stress and resulted in
anisotropy of the viscosity, even in relatively pure layered
rock salt (Adamuszek et al., 2021). Despite the impact of
interbeds on the rock salt strength and deformation
properties, numerical simulations have indicated that rock
salt caverns with high interlayer content have better
stability performance than those with lower or no
interlayer content, but they have a smaller available
volume because of the collapsed interbed sediments at the
cavern bottom from the construction (Zhang, Liu,
et al., 2021).
Shearing experiments of mixed halite‐calcite layers
F I G U R E 9 Rock salt samples with impurities, (a) bedded rock salt,
revealed that bimineralic shear zones at large shear
(b) rock salt with distributed impurities. Figure modified from strains are primarily controlled by the weaker compo-
(Cyran, 2021). nent, halite (Kawamoto & Shimamoto, 1998). Similar
observations were made for anhydrite‐halite mixtures Impurities also have a significant impact on the
(Ross & Bauer, 1992). However, torsional deformation geomechanical behavior of rock salt in cyclic experi-
experiments on halite‐calcite mixtures demonstrated that ments. Discontinuous fatigue tests have time intervals
the strength of the two‐phase mixtures was higher than where the stress remains constant, and this leads to faster
pure halite, and that the calcite grains hindered halite plastic deformation and a reduction in the fatigue life.
plastic flow and stress relaxation (Marques et al., 2010). This behavior is caused by the internal residual stress
Moreover, another study on the mechanical properties between defects and the host material, and the residual
and gas permeability of rock salt showed that the stress is greater for a larger difference in the elastic
impurity content results in an increase of the rock salt modulus of the impurity and the host material (Fan
strength, and a higher permeability (Zhang, Liu, et al., 2020) (Figure 10).
et al., 2020).
A study by Speranza et al. (2016) linked natural
heterogeneities and the “maturity” of rock salt to 6 | U N D E R G R O N D GA S S T O R A G E
rheological properties and concluded that rock salt IN ROCK SALT CAVERNS
type, that is, textural characteristics, mineralogical
properties and fluid inclusion type and abundance, 6.1 | Rock salt cavern construction methods
needs to be taken into account in studies and designs
for rock salt applications. The rheological behavior of Caverns can be made artificially in rock salt by salt solution
rock salt is impacted by impurities (solid inclusions) in mining, which involves dissolving salt with water and
halite through high rates of creep due to accelerated pumping the brine back up to the surface (Figure 11). For
diffusion rates at halite‐solid phase interfaces (Závada caverns in halite, one cubic meter of rock can be dissolved
et al., 2015). Laboratory studies on potash investigat- with seven to eight cubic meters of fresh water pumped into
ing the effect of mineralogical composition to geome- the cavern. Accelerated rock salt leaching is achieved by the
chanical properties showed that elastic constants and use of high‐pressure water jets with water stream pressure of
dilational properties of the potash are independent of 500 bar (Korzeniowski et al., 2020). The rock salt dissolution
mineralogical content, whereas the creep properties are in dynamic water and the fluid transport mechanism during
directly correlated to the mineralogical content, solution mining have been modeled based on kinetics of the
although grain size, porosity and pre‐existing micro- convection‐diffusion process and the theory of fluid dynam-
fractures were not accounted for (Mellegard ics and chemical kinetics (Yang & Liu, 2017). In the solution
et al., 2012). The impact of heterogeneity in Zechstein mining under gas method for the construction of salt
rock salt on geomechanical properties has also been caverns, a protective fluid (blanket), that is insoluble in
reported by Wilkosz et al. (2012) and their results water, lighter than water and unreactive with water or salt) is
indicate a potential dependence of rock salt strength used to protect the casing shoe and to control the cavern
and creep rate on subgrain occurrence in halite. shape (Sedaee et al., 2019). Commonly, liquid hydrocarbons
Synthetic rock salt samples produced with sodium are used as blankets (Favret, 2004), but due to their cost and
sulfate and gypsum impurities were also used for environmental concerns, nitrogen gas has been studied for its
geomechanical analysis and showed that a higher use as a blanket for the construction of a rock salt cavern for
content of impurities led to a decrease in the strength underground gas storage, and optimized leaching parameters
of the rock salt samples (Liu, Zhang, Fan, can be predicted with simulation of water injection and
Zuo, et al., 2020). Not only second phase particles in nitrogen gas injection pressure (Wang et al., 2021). In
rock salt but also solid solution impurities impact its bedded salt, where the caverns have greater horizontal
deformation properties, as is documented by Heard dimensions, solution mining with double‐well convection is
and Ryerson (1986). employed (Zhang, Wang, et al., 2020).
F I G U R E 10 Simulation geometric model with Fax the axial force, Pc the confining stress and D the impurity diameter, and the variation in
residual stress variation with different maximum applied external stress with Pk the peak axial stress, modified from Fan et al. (2020).
The rate of cavern closure is strongly dependent on grain

size, with much higher rates for fine grained rock salt
caused predominantly by pressure solution creep (Cornet
et al., 2018). Caverns at shallower depths may be prone to
catastrophic failure. Models have shown that collapse
depth does not increase linearly with the burial depth.
Therefore, collapses of rock salt caverns generally happen
at depths shallower than 600 m (Zhang, Wang, et al., 2018).
In rock salt layers at depths of more than 900 m, there are
common issues with shaft lining deformation, and
recently, a new methodology involving local and con-
trolled leaching to remove the excessive creep into the
outbreak side of the shaft diameter has been proposed
(Kaminski, 2021). Besides the cavern depth, the pressure
and temperature gradients of the overburden, the pressure
inside the cavern, the shape of the cavern and the rock salt
properties such as grain size and moisture content will also
F I G U R E 11 Schematic of salt solution mining process with the influence the rate of creep deformation. Caverns with
production of a salt cavern. irregular shaped walls show a lower shrinkage in volume
and less displacement of the cavern walls (in comparison
to regular shaped salt caverns). Larger plastic deformation
6.2 | Rock salt mineralogy and cavern in these caverns is located to their overhanging and
construction concave parts (Liu, Zhang, Fan, Jiang, et al., 2020).
Numerical simulations have indicated that ellipsoid
Salt solution mining generally targets thick rather homoge- shaped caverns are more stable than cylindrical or cuboid
neous halite formations. Rock salt existing in diapirs is shaped caverns, and that the roof shape (which should be
therefore preferred over bedded salt formations. The designed as an arch) is more important than the shape of
composition and heterogeneity of the rock salt is important, the side walls with regard to the stability of the caverns
since differences in dissolution behavior will influence the (Liu, Zhang, Fan, Jiang, et al., 2020). Physical simulation
shape of the cavern, and cause potential collapse of less technologies and testing systems of single‐well solution
soluble components, such as anhydrite or dolomite. mining in rock salt have been developed for cavern shape
Moreover, as is shown by the studies on underground gas control (Wang, Wang, et al., 2022).
storage in rock salt caverns in China, the bedded rock salt
nature with interlayers of anhydrite, glauberite and mud-
stone leads to collapse and piling up of insoluble mudstone 6.4 | Geomechanical properties of rock salt
at the bottom of the cavern during salt solution mining, thus caverns for gas storage
causing a one‐third or even two thirds reduction of the gas
storage capacity of the cavern (Li et al., 2016). Moreover, the Beyond the purpose of the production of salt from salt
mudstones are volumetrically expanded after collapse in the solution mining, the rock salt caverns can serve as
cavern due to clay swelling, an increase in the volume storage containers for hydrocarbons and waste. More-
of the pore space free water, and water bound to the surface over, rock salt caverns have gained great attention
of the particles (Yao et al., 2022). Apart from the geological recently in the renewable energy field as potential
characteristics, the construction technology and tubing storage sites for hydrogen (AbuAisha & Billiotte, 2021)
failure are also considered as factors that can lead to the or compressed air (Khaledi et al., 2016). A brief
formation of irregular caverns, and their operation comes overview of the history of storage of fluids and gases
with risks and safety hazards (Xue et al., 2020). Further- in underground salt caverns is presented in Firme et al.
more, solution mining simulation models have shown that (2019). The development of an underground cavity
creep deformation induced volumetric shrinkage and results in a response of the surrounding rock, which
displacement of the cavern roof stabilizes at a length of expands into the newly created void volume, and thus
600 m (or at a length‐to‐diameter ratio of around 5 to 6) for inelastic dilatation (volume expansion) occurs. The
horizontal cavern structures in bedded salt formations (Li, latter triggers a decrease in fluid pressure, which may
Zhang, et al., 2022). result in the generation of a gas‐fluid (two‐phase) system
(Beauheim & Roberts, 2002). With small amounts of
dilation (≥0.05 vol%) sufficient microfractures form to
6.3 | Rock salt cavern depth, shape, create an interconnected pore network beyond the
and microstructures percolation threshold (Peach, 1991). Hence, dilation
around an underground void volume can cause halite to
Generally, rock salt caverns are made through solution shift from practically nonexistent permeability to
mining in formations at depths between around 200 and measurable permeability. Moreover, dilatancy, and thus
2000 m. Greater depths would lead to significant creep permeability, is enhanced by second phase impurities in
and cavern closure, as a larger pressure difference causes a the halite such as anhydrite and clay (Beauheim &
greater cavern shrinkage rate (Zhang, Wang, et al., 2018). Roberts, 2002). Permeability, which is a key factor in
predicting the integrity of the storage site, is not simply temperature will also be affected by repeated injections
a function of stresses or strains. It is a very nonlinear and withdrawal of gas in rock salt caverns. The injected
function of dilatancy, impacted by microcrack linkage compressed gas is generally cooler than the temperature
(Popp et al., 2001), and it is strongly dependent on the of the rock salt enclosing the cavern. Moreover, a rapid
type of salt. Nevertheless, the dilatancy boundary is gas pressure drop in the cavern results in cooling, and
considered a safety boundary for permeability and thus thermal contraction of the rock salt, causing tensile
integrity (Hunsche & Hampel, 1999). stress (Bérest et al., 2007). Studies on high frequency
In the context of renewable energy storage, rock salt cycling of salt caverns have indicated that thermally
caverns provide a solution to deal swiftly with peak induced tensile fracturing is possible, and thermo‐
demand and demand fluctuations. The caverns enable mechanical modeling can help predict the location,
rapid cycling with a 15 min's withdrawal to injection orientation, and timing of the first fractures (Blanco‐
changeover time. Such caverns for storage are generally Martín et al., 2018). Studies on permeability evolution
at a depth of 1 to 2 km below the surface, and about in rock salt have shown that dynamic mechanical and
110 m below the top of the salt formation. It is best to thermal fatigue may lead to a slight increase in
use rock salt caverns in diapirs for gas storage rather permeability due to microcracking and a reduction in
than bedded rock salt, since the interface between permeability during static fatigue (creep) due to self‐
different lithologies may be a potential leakage site, and healing (Grgic et al., 2022). The mechanisms behind
a focus location for strain weakening, for example, weak self‐healing of damage in rock salt involve mechanical
interfaces between rock salt and mudstone beds (Zhang closure, diffusive healing driven by a reduction in
et al., 2014). Injection and withdrawal of gas results in surface energy, and healing by recrystallization; and
pressure cycling. Large stress cycles can lead to inelastic the influencing factors include stress, temperature,
deformation around salt cavern walls and trigger the initial damage, humidity, and chemical environment
development of grain boundary cracking and frictional (Kang et al., 2019). The effects of the tempo‐spatial
sliding enabling the redistribution of water and poten- variation of temperature and pressure (Figure 12) on
tially initiating viscous processes (Ding et al., 2021). the mechanical behavior of the cavern have also been
Instability of cavern walls could be caused by the simulated using a coupled aero‐thermo‐mechanical
production of linked arrays through the linkage of model (Li et al., 2023). Monitoring of acoustic emis-
preferentially opened grain boundaries with shear sions was also employed to investigate the impact of salt
slipping boundaries (Ding et al., 2017). Large stress cooling related to fast injection and withdrawal cycles.
cycling should thus be avoided, and holds could be Studies have shown that the first cooling period displays
employed to allow stress relaxation and healing of the strongest and deepest acoustic emissions (Balland
cracked grain boundaries (Ding et al., 2021). The et al., 2018). If the cavern is not used for a long time, the
F I G U R E 12 The variation of temperature and pressure in a rock salt cavern through time and space, adapted from W. Li et al. (2023).
temperature inside the cavern will increase, resulting in in bedded rock salt, and on potential collapse and
higher pressure. leakage in bedded rock salt in the context of under-
ground gas storage.
Despite these efforts, more research is required on the
7 | CONCLUSION understanding of the impact of impurities (type, quantity,
etc.) on rock salt geomechanical behavior. Given that rock
This review provides a generic introduction to rock salt salt geomechanical properties are critical inputs for numeri-
mineralogy, microstructures and geomechanical propert- cal models used for cavern stability calculations at the
ies, as well as methods to investigate such properties. design, completion and operation stage, and risk assess-
Rock salt studies have gained much interest over the last ments, it is of huge importance that representative values
few years due to its potential as underground storage should be used for the different rock salt properties. Some
sites for hydrogen and methane to satisfy peak demand recent efforts have been put in deriving a constitutive model
and changes in renewable energy input from solar and for rock salt with impurities using a two‐phase material
wind. The safety of those storage sites needs to be approach. However, this would need to be further refined
guaranteed. Given the wide variety of rock salt miner- and extended using a multiphase material approach with
alogies and microstructures linked to the depositional adequate rheological considerations. In the context of tests
environment, diagenesis and geological and structural on synthetic rock salt samples, the preparation methods with
history, the influence of mineralogical, geochemical and controlled type and distribution of impurities need further
microstructural characteristics on the geomechanical improvement to better reflect the geological conditions and
properties and potential porosity or permeability changes natural mechanical interactions between halite and impurity
of the walls of rock salt caverns needs to be well particles.
explored. It is clear that impure anhydrite, clay, or even Another aspect that needs to be considered in
bedded salt formations behave geomechanically differ- future research is the potential impact of the edges of
ently from the purer halite. Furthermore, cyclic loading rock salt domes and related rock salt fabrics. Although
tests are important to simulate repeated gas injection and bedded salt has received increasing attention over the
extraction. last few years, the effect of the rock salt setting, such as
domal salt, diapir, bedded salt, and the position within
those environments (e.g., near the edge of the salt
8 | RESEARCH TREND A ND dome) on the geomechanical properties of the rock salt
FUTURE PERSPECTIVES has not been studied much yet. An improved under-
standing of rock salt setting and related rock salt
In the past 5 to 10 years, the interest in underground rock fabrics, heterogeneity, impurities, and so forth, and the
salt caverns has exponentially increased. This is mainly link with geomechanical properties is important for
triggered by the transition to renewable energy, accom- wider rock salt exploration, and improved predictions
panied by the need for energy storage, like the storage of on feasibility and stability of rock salt caverns
hydrogen. Moreover, the demand for energy increases, development, and risk assessment for underground
and thus rock salt formations are more widely explored gas storage in such caverns.
for the construction of underground caverns. This Moreover, further research is needed regarding the
evolution has caused the following trends in rock salt assessment of stability of rock salt caverns. A better
research in the past 5 to 10 years. understanding of the process and mechanisms of
The most important trend is the focus on understanding damage and cavern roof collapse is required through
the rock salt geomechanical behavior under dynamic, cyclic consideration of the effect of interactions between fluid
or multistage loading rather than static or single‐stage and solid phases. In terms of cavern geometry,
loading. This trend is clearly associated with the intended simulations need to be further developed based on
purpose of using rock salt caverns for energy storage with the actual variations in internal gas pressure within
repeated injection and withdrawal of gas. In addition to rock specific caverns, and improved algorithms need to be
salt creep deformation models derived from long‐term established for optimization of cavern shape for
deformation under static loads, fatigue behavior (linked to underground gas storage.
cyclic loading), and in particular combined fatigue and creep With regard to the creep model, additional parame-
deformation, are studied. Moreover, studies with geomecha- ters, as mentioned earlier, may need to be considered to
nical tests on rock salt samples involve a wider range of capture such complex mechanism more realistically. At
methodologies, including for example micro‐CT to visualize the same time, the models should remain relatively
pores and mineral heterogeneity in three dimensions, and simple so as to be used in engineering practice, preferably
thus enabling reconstruction of microstructural deformation being applicable, apart from soft rocks, to a wide range
mechanisms. Besides experimental tests, wide attention has of rock types.
been paid to establishing the nonlinear creep damage model.
Another important focus in recent literature on rock CONF LICT OF INTEREST ST ATE MENT
salt involves the study of bedded rock salt, or rock salt The authors declare no conflict of interest.
with impurities. Because of the wider need of rock salt
caverns, exploration needs to be extended beyond the DA TA AV AI LA BI LIT Y S TA TEME NT
high‐purity rock salt. There is an increase in studies on This is a review paper, and data mentioned can be found
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113523. Veerle Vandeginste is a professor in the
Závada P, Desbois G, Urai JL, et al. Impact of solid second phases on Department of Materials Engineering at
deformation mechanisms of naturally deformed salt rocks (Kuh‐e‐ KU Leuven (Belgium). She has a PhD in
Namak, Dashti, Iran) and rheological stratification of the hormuz
salt formation. J Struct Geol. 2015;74:117‐144.
Geology from KU Leuven (Belgium),
Zhang DM, Agostini F, Jeannin L, Skoczylas F. New insights brought and worked at the Geological Survey of
by micro‐tomography to better understand gas transfer property Belgium, and then at CEREGE
variation and coupling effects in salt rocks. Rock Mech Rock Eng. (France). She joined the Department of Earth Science
2021;54(12):6457‐6480.
Zhang G, Li Y, Yang C, Daemen JJK. Stability and tightness
and Engineering at Imperial College London in 2009,
evaluation of bedded rock salt formations for underground gas/ and in 2012, she became an independent research
oil storage. Acta Geotech. 2014;9(1):161‐179. fellow. In 2015, she was appointed as an assistant
Zhang G, Wang Z, Zhang K, et al. Collapse mechanism of the professor at the University of Nottingham, where she
overlying strata above a salt cavern by solution mining with established the Geochemistry research discipline in
double‐well convection. Environ Earth Sci. 2018;77(16):588.
Zhang GM, Wang W, Liu J, et al. Stability of the bedded key roof
the School of Chemistry, and was promoted to
above abandoned horizontal salt cavern used for underground gas associate professor in 2020, and then returned to
storage. Bull Eng Geol Environ. 2020;79(8):4205‐4219. KU Leuven (Belgium). Her research motivation is
Zhang JJ, Wei CT, Vandeginste V, et al. Experimental simulation study driven by the challenges of finite resources and global
on water migration and methane depressurizing desorption based warming. Her research focuses currently on physical
on nuclear magnetic resonance technology: a case study of middle‐
rank coals from the panguan syncline in the Western Guizhou
chemistry of material interfaces and their link to
Region. Energy Fuels. 2019;33(9):7993‐8006. material behavior.
Zhang JJ, Wei CT, Chu XX, Vandeginste V, Ju W. Multifractal analysis
in characterizing adsorption pore heterogeneity of middle‐ and
Yukun Ji graduated in 2014 as a civil
high‐rank coal reservoirs. ACS Omega. 2020;5(31):19385‐19401.
Zhang Q, Wang JB, Song ZP, Feng SJ, Zhang YW, Zeng T. Microstructure engineer and obtained his PhD degree in
variation and empirical fatigue model of salt rock under cyclic loading. geotechnical engineering in 2019 at
Rock and Soil Mechanics. 2022;43(4):995‐1008. China University of Mining and Tech-
Zhang QX, Liu J, Wang L, et al. Impurity effects on the mechanical
nology (won Excellent Civil Engineering
properties and permeability characteristics of salt rock. Energies.
2020;13(6):1366. doi:10.3390/en13061366
Graduate Award in Jiangsu Province).
Zhang X, Liu W, Jiang D, et al. Investigation on the influences of Then, he joined the School of Chemistry at University
interlayer contents on stability and usability of energy storage of Nottingham in 2019, and he was also promoted to
caverns in bedded rock salt. Energy. 2021;231. doi:10.1016/j. research fellow in 2019. Since June 2021, he is an
energy.2021.120968 associate professor in Geotechnical Engineering at
Zhang ZX, Liu W, Guo Q, Duan XY, Li YP, Wang TT. Tightness
evaluation and countermeasures for hydrogen storage salt cavern
China University of Mining and Technology, where
contains various lithological interlayers. J Energy Storage. he contributes teaching and researching in under-
2022;50. doi:10.1016/j.est.2022.104454 ground energy storage, water rock interaction, and
Zhao J, Zhang Y, Zhang M, et al. Research on micro‐pore structure multifield coupling model.
and 3D visual characterization of inter‐salt shale based on X‐CT
imaging digital core technology. Processes. 2022;10(7):1321.
doi:10.3390/pr10071321
Zhao K, Ma H, Liang X, et al. Damage evaluation of rock salt
under multilevel cyclic loading with constant stress intervals
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2022;208. doi:10.1016/j.petrol.2021.109517 microstructures and geomechanics of rock salt for
Zhao Y. Experimental study on the dilatancy of rock salt from an underground gas storage. Deep Underground Sci
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doi:10.1002/dug2.12039

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Received: 23 December 2022 | Revised: 15 February 2023 | Accepted: 13 March 2023

Mineralogy, microstructures and geomechanics of rock salt

Veerle Vandeginste1 | Yukun Ji2 | Frank Buysschaert3 | George Anoyatis4

Funding information Highlights

1 | INTRODUCTION are commonly mined and used in many industrial

Deep Underground Sci and Eng. 2023;2:129–147. wileyonlinelibrary.com/journal/duse | 129

(Warren, 2006). The variation in salt mineralogy is linked

Acoustic emission (AE) is a common method applied

expressed as the sum of the strain rate caused by

where A and B denote constants related to deformation

The rate of cavern closure is strongly dependent on grain

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