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Geology

Nanograins form carbonate fault mirrors

Shalev Siman-Tov, Einat Aharonov, Amir Sagy and Simon Emmanuel

Geology 2013;41;703-706
doi: 10.1130/G34087.1

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Nanograins form carbonate fault mirrors
Shalev Siman-Tov1, Einat Aharonov1, Amir Sagy2, and Simon Emmanuel1
1
Institute of Earth Sciences, The Hebrew University of Jerusalem, Jerusalem 91904, Israel
2
Geological Survey of Israel, 30 Malkhe Israel, Jerusalem 95501, Israel
ABSTRACT
Many faults are characterized by naturally polished, reflective,
glossy surfaces, termed fault mirrors (FMs), that form during slip.
Recent experiments also find that FMs form during rapid sliding
between rock surfaces, and that FM formation coincides with pro-
nounced friction reduction. The structure of FMs and the mecha-
nism of their formation are thus important for understanding the
mechanics of frictional sliding, particularly during earthquakes.
Here we characterize the small-scale structure of natural carbonate
FMs from three different faults along a tectonically active region
of the Dead Sea transform. Atomic force microscopy measurements
indicate that the FMs have extremely smooth surface topography,
accounting for their mirror-like appearance. Electron microscope
characterization revealed a thin (<1 µm) layer of tightly packed
nanoscale grains coating a rougher layer comprising micron-size
calcite crystals. The crystals contain closely spaced, plastically
formed twins that define new subgrain boundaries. The narrow sub-
grains are observed to break into submicron pieces near the sheared
surface. This observation suggests a new brittle-ductile mechanism
for nanograin formation. The role of ductility during frictional slid-
ing, both in forming the nanograin layer, and in the deformation
process of the powder, may be critical for understanding shear on
geological faults.
INTRODUCTION
Fault mirrors (FMs) are typical of many fault surfaces, and appear
in a variety of tectonic environments and rock types (Hancock and Barka,
1987; Jackson and McKenzie, 1999; Power and Tullis, 1989). These natu-
rally polished fault surfaces are a form of slickensides that is characterized
by high visible-light reflectivity (Fig. 1). Because FMs are well-defined
slip surfaces, ubiquitous in shear zones, they have often been examined
in case studies of fault surfaces at various scales; however, their polished
nature has often been overlooked.
The structure and roughness of natural slip surfaces have been stud-
ied in detail over the last few decades, in both silicate and carbonate rocks
(e.g., Power and Tullis, 1989; Smith et al., 2011). Previous studies have
Figure 1. Glossy, mirror-
like strike-slip fault sur-
face in brecciated Eo-
cene limestone at Kfar
Giladi quarry, Israel.
GEOLOGY, June 2013; v. 41; no. 6; p. 703–706; Data Repository item 2013193 | doi:10.1130/G34087.1
GEOLOGY | JuneSociety
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America. For permission to copy, contact Copyright Permissions, GSA, or editing@geosociety.org.
suggested that surface topography obeys a self-affine roughness ranging
in scale from microns to kilometers (Candela et al., 2009; Power et al.,
1987). However, FM scales smaller than 1 µm have not so far been stud-
ied, although roughness at such small scales is likely to be critical for both
the optical and frictional characteristics of these smooth surfaces.
For a surface to be glossy and reflect light specularly, like a mirror, it
must obey the Rayleigh roughness criterion (Beckmann and Spizzichino,
1963):
λ
A< , (1)
16 cos θ
where A is the mean roughness amplitude of the surface, θ is the angle
of incident light, equal to the angle of specular reflection (measured rela-
tive to the surface normal), and λ is the light wavelength. In the case of
scale-dependent surface roughness, this criterion must be obeyed at least
at lateral scales, l, shorter than λ. Therefore, if a surface is observed at
0° < θ < 70°, under visible light (λ = 550 nm), and appears glossy, this
indicates that A < ~100 nm at least for lateral scales l < 550 nm.
Extreme nanoscale smoothness may reduce friction, as observed in
sliding experiments on very smooth surfaces (Byerlee, 1967; Hayward et
al., 1992). FMs were recently observed to form during experiments involv-
ing rapid, earthquake-like slip between rock surfaces, and their formation
was suggested to coincide with friction reduction (Han et al., 2011; Smith
et al., 2013). Both in engineered surfaces and in natural faults the forma-
tion of mirror-like surfaces is of extreme interest; however, the structure
of FMs, their mechanism of formation, and their impact on frictional slid-
ing are unclear. This paper characterizes the small-scale structure of natu-
ral carbonate FMs from three different faults along a tectonically active
region of the Dead Sea transform, shedding light on possible formation
mechanisms of FMs.
METHODS
Hand samples were taken from three well-preserved carbonate FMs
related to the Dead Sea transform (Fig. DR1 and Table DR1 in the GSA
Data Repository1): the Kfar Giladi fault (KGF), the Nahal Avinadav fault,
and the Yair fault. For comparison, a fault surface that is not mirror like,
from the Nahal Uziyahu fault, was also examined (Fig. DR2).
High-resolution techniques were used to characterize the structure
and quantify roughness of FMs on scales ranging between 0.01 µm and
1000 µm. Surface topography was scanned using an optical profilometer
on the micron scale and atomic force microscopy (AFM) down to the
submicron scale. Surface structure was also studied with scanning elec-
tron microscopy (SEM). A cross-sectional foil, prepared by the focused
ion beam technique, was studied using transmission electron microscopy
(TEM) (see the expanded Methods section in the Data Repository).
RESULTS
At the outcrop scale (Fig. 1) the FMs are composed of a thin
(~10−2 m) ultracataclasite layer, which in general appears very smooth
and hard. At these large scales, corrugations and surface undulations
have 0.1–1 m wavelengths. Surprisingly, from the hand-sample scale
to ~1 µm, many surfaces appear very smooth (Fig. 2A) with few minor
1
GSA Data Repository item 2013193, detailed geological settings, expanded
methods, and additional power spectral density analysis, is available online at
www.geosociety.org/pubs/ft2013.htm, or on request from editing@geosociety.org
or Documents Secretary, GSA, P.O. Box 9140, Boulder, CO 80301, USA.
| Published online 16 April 2013
703
 Downloaded from geology.gsapubs.org on October 16, 2014
Figure 2. Atomic force microscopy (AFM) and scanning electron mi-
croscopy scans of fault mirrors. A: AFM scan of fault surface from
Yair fault, Israel. Darker colors represent lower regions; brighter col-
ors represent higher regions (see gray-scale bar). Surface is very
flat except for several scratches and few prominent grains (seen
as white blotches). B: One-dimensional profile from surface (white
dashed line in A) demonstrates flatness, scratches, and grains. C:
Closeup of smooth region (black rectangle) shows typical ampli-
tudes <20 nm. D: Micron-size parallel striations at Kfar Giladi quarry.
Rougher, nonstriated regions are exposed micron-size calcite crys-
tals of original rock. E: At submicron scale, fault mirror material of
Kfar Giladi fault (KGF) is composed of packed rounded nanograins;
no scratches are observed. F: Nahal Avinadav fault material shows
characteristics similar to those of KGF material.
grooves; subparallel striations (Fig. 2D), which are typically found on
many slip surfaces, were infrequently observed. The few striations that
were observed were oriented mostly parallel to the long axis of the cor-
rugations (Sagy and Brodsky, 2009). In contrast, we found Reidel shears,
branching from the FMs, covered by prominent striations. One difference
between the Riedel shears and the FMs is the possibly different amount of
slip on the surfaces. Previous studies found that roughness decreases with
increasing slip (Sagy et al., 2007).
At scales smaller than ~1 µm, SEM and AFM images reveal a dif-
ferent picture. Instead of a relatively planar surface with a few minor
grooves (Fig. 2A), the surface is composed of particles with diameters of
tens to hundreds of nanometers; no small-scale striations or grooves are
observed (Figs. 2E and 2F). Similar images were found in high-velocity
shear experiments on limestones (Tisato et al., 2012).
In order to quantify the observed scale-dependent geometry, power
spectral density (PSD) analyses of surface roughness were performed
(Sagy and Brodsky, 2009). Mean PSD values were obtained by averag-
ing the PSD of each of the 512 AFM and ~550 profilometer profiles for
slip-parallel and slip-perpendicular directions. Figure 3A plots the mean
PSD versus wavelength for the KGF for nearly five orders of magnitudes
(see Fig. DR4 for PSD analyses for the Yair and Nahal Avinadav faults).
For self-affine surfaces, the PSD is expected to scale as a power law
of the wavelength, producing a constant slope on a log-log plot over a
wide range of scales. In self-affine surfaces when the horizontal direction
x is viewed at magnification λ, the vertical direction z must be magnified
by λH in order to maintain scale invariance, such that δx → λδx, δz →
λHδz, where H is the Hurst exponent (Barabási and Stanley, 1995). The
Hurst exponent is related to the PSD slope β via H = (β − 1)/2. Figure 3A
shows that the slope is not constant, but instead steepens for decreasing
wavelengths. Therefore, the measured surfaces are not self-affine at all
the scales measured here; i.e., at the nanoscale, FMs are smoother than
would be expected from extrapolation based on the self-affine behav-
ior observed in previous studies of larger scales (Renard et al., 2006;
704
Figure 3. Surface roughness analysis for a fault mirror surface from
Kfar Giladi quarry, Israel. A: Power spectral density (PSD) analysis
based on three atomic force microscopy (AFM) scans (1, 10, and 100
μm side width), and one profilometer scan. Blue points are analysis
results of slip-perpendicular profiles; red points are results of par-
allel profiles. Four colored lines are drawn above data points, with
slopes β = 1.6, 2.4, 3, and 4, corresponding to Hurst exponent H =
0.3, 0.7, 1, and 1.5, respectively, illustrating that slope steepens with
decreasing wavelength. B: Root mean square (RMS) analysis of sur-
faces from Kfar Giladi fault (KGF; lower curve, x), and Nahal Uziyahu
fault (upper curve, squares), using AFM 10 µm scan width. Gray box
marks region that obeys Rayleigh roughness criterion. KGF surface
obeys this criterion and is reflective, while the non–fault mirror sur-
face of Nahal Uziyahu fault is outside this region.
Candela et al., 2009). Such scale dependence in the PSD curve, together
with the clear morphological differences observed at the nanoscale, sug-
gests a fundamental scale-dependent structural difference. In addition,
the typical roughness anisotropy between slip-perpendicular and slip-
parallel directions (Power et al., 1987; Renard et al., 2006) is absent
here (Fig. 3A). This may not be surprising, because our measurements
focused on naturally polished non-striated mirror surfaces (Figs. 1 and
2A).
In addition to the power spectral density analysis, root mean square
(RMS) analysis (Candela et al., 2009), which provides an approximation
for the roughness amplitude, was performed on the topography of two
fault samples (Fig. 3B; Fig. DR2). Figure 3B shows, as expected, that
RMS increases with increasing lateral scale of measurement, l. According
to the roughness criterion, a surface is reflective if undulations at scale l <
550 nm have amplitudes <100 nm. For the KGF, both the topography pro-
files (similar to those observed at Yair fault shown in Figures 2B and 2C)
and the RMS values show roughness <20 nm at l ~ 550 nm, explaining
the high reflectivity of the surface. In contrast, the Nahal Uziyahu fault, a
non-FM surface, shows RMS values >100 nm at l ~ 550 nm, explaining
its poor reflectivity.
In order to further investigate the scale-dependent structural differ-
ence detected in Figure 3, we probed the KGF interior (i.e., the subsur-
face) using bright-field TEM images (Viti, 2011) of the cross-section foil
(Fig. 4A). Two distinct layers, separated by a rough boundary, are found
beneath the FM: an outermost layer composed of nanograins (Fig. 4B),
and a deeper layer consisting of micron-size calcite crystals (Fig. 4C). The
nanograin layer comprises highly packed particles with diameters of tens
to hundreds of nanometers and has a variable thickness of <1 µm. No pref-
erential orientation is observed in the particles. Chemical analysis and dif-
fraction patterns indicate that the layer is composed of calcite nanograins
surrounded by a matrix comprising mainly silicon and aluminum. By con-
trast, the deeper layer consists entirely of micron-size calcite crystals, with
pores observed along crystal boundaries (Fig. 4C). The calcite crystals
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Figure 4. Cross section of Kfar Giladi quarry, Israel. A: Transmis-
sion electron microscope image of foil showing two different lay-
ers, outer (B in white box) and deeper (C in white box), separated
by rough (black dotted) line. Outer layer comprises nanograins and
determines surface tiny roughness. B: High-resolution image of
outer layer, which comprises highly packed rounded nanograins (50
nm white scale bar, marked by black arrow, indicates particle diam-
eter) with no observed preferred orientation. Lighter homogeneous
solid line represents carbon and platinum (Pt) sample coatings.
C: High-resolution image of deeper layer. Microcalcite crystals are
twinned (100 nm black scale bar, marked by white arrow, indicates
twin width) and pieces of beam-like subgrains have broken to form
nanograins (marked by black ellipses). D: Schematic illustration of
A. Deeper layer comprises twinned calcite crystals (twins drawn as
gray parallel bands), while outer layer comprises nanograins that
cover rougher surface of large crystals and smooth fault surface.
At least some nanograins form by breaking of beam-like subgrains,
defined by twins within crystals (circular inset).
comprise a series of parallel bands, reflecting subgrain boundaries prob-
ably formed by mechanical twinning. In some pores, tiny sections of the
twinned crystals are observed, presumably broken off from much larger
subgrains (black ellipses in Fig. 4C).
Our analysis of FMs implies that both their roughness and structure
change critically at the submicron scale. At this small scale, the FMs do
not follow the self-affine behavior and striations are not observed, which
contrasts with previous observations at larger scales. Instead the FMs are
extremely smooth, conforming to the Rayleigh roughness criterion. The
deep grooves (hundreds of nanometers; Figs. 2A and 2B) do not signifi-
cantly reduce this extreme reflectivity as they represent only a small por-
tion of the total surface area. Thus, we suggest a rule of thumb for esti-
mating fault surface roughness in the field: an FM implies that the mean
roughness, A, at least for lateral scales below 550 nm, is <100 nm.
GEOLOGY | June 2013 | www.gsapubs.org
DISCUSSION AND CONCLUSIONS
Formation of Naturally Polished Surfaces
Natural FMs may be formed by processes similar to those that facili-
tate the fabrication of mirror-like surfaces in industrial polishing (Ada-
chi and Kato, 2000). A typical industrial polishing process involves three
stages: (1) brittle abrasion during which the overall roughness is reduced
by removing surface asperities, although striations are often formed; (2)
reduction of wear particle sizes and formation of a nanograin layer; and (3)
formation of smooth hard surfaces within the nanograin layer by smear-
ing and sintering of the nanograins. Ultimately, brittle scratches on the
surface are filled by nanograins, resulting in roughness amplitudes <100
nm. Similarly, our observed natural FMs have features that are consistent
with these three stages (Fig. 4), as do fault mirrors formed in experimental
shearing of rocks at high shear rates (Han et al., 2011; Hirose et al., 2012;
Smith et al., 2013).
Formation of Nanograins by Plastic-Brittle Deformation
Although nanograins have been previously observed in fault rocks
(Chester et al., 2005; Power and Tullis, 1989; Viti, 2011; Wilson et al.,
2005) and in shear experiments (Han et al., 2010; Tisato et al., 2012),
their origin is debated. The difficulty in explaining the formation of
nanograins arises because a fragmentation process due to Griffith cracks
is not expected to form particles smaller than ~1 μm. Instead, at scales
below this grinding limit, plasticity is expected to dominate deformation
(Sammis and Ben-Zion, 2008). As a result, different mechanisms have
been proposed to explain formation of nanograins in general and in faults
in particular (Han et al., 2010; Koch, 1997; Sammis and Ben-Zion, 2008):
(1) mineral decomposition during shear heating; (2) rapid solidification
from melt caused by shear heating; (3) crystallization of amorphous
phases; (4) brittle fracturing by tensile shock loading near a propagating
fault tip associated with seismic motion; and (5) subcritical crack growth.
An additional mechanism that is often used in industrial pro-
cesses to produce nanograins and that does not need high temperatures
invokes mechanochemical effects obtained by mechanical milling. Mill-
ing involves repeated grain impacts, producing numerous crystal defects
that form nanoscale grain boundaries. When subjected to further shear a
nano powder forms from the grains (Koch, 1997). The TEM images in
our study suggest that nanograins may form in a two-step process similar
to mechanical milling: (1) strain-induced plasticity in crystals, that creates
long beams, and (2) beam breaking by brittle fracture (Fig. 4D). As twin
formation introduces anisotropy, Griffith’s criterion no longer holds and
the fracturing of crystals at very small scales becomes easier; the length
scale of particles formed during this stage is determined by the width of
the twins (50 ± 30 nm).
Formation of crystal defects and nanograins by milling occurs both
at high and low strain rates: twins are sometimes thought to indicate slow
strain rates, yet they also form during calcite fracturing (Dickinson et al.,
1991) and at high-shear-rate experiments in carbonates (Han et al., 2010).
Han et al. (2010) found crystals with dense mechanical twinning border-
ing the slip zone, similar to natural FMs, suggesting that milling may have
operated concurrently with decarbonation to form nanograins, in a com-
bined formation process that could also operate in natural FMs. Shen et al.
(1995) showed that milling produces nanograins at loading and unload-
ing times of ~10−5 s. At the other end of the slip-rate scale, creep rates
much below seismic slip velocities are also observed to form nanograins
by mechanical milling (Tisato et al., 2012).
Ductile Deformation within the Nanograin Layer
Once the nanograin layer is in place, and assuming shear localizes
upon it (e.g., Chester et al., 2005), several observations point to the impor-
tant role that ductility plays in its subsequent deformation. (1) Scratches
are observed at scales larger than 1 µm (Fig. 2A), but disappear at the
705
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submicron scale (Figs. 2E and 2F). This may be explained via the grind
limit; i.e., grains <1 µm do not scratch the surface, but instead deform
plastically. (2) Nanograins are mostly rounded, and since fracturing is not
expected to occur at submicron scales, the rounding is best explained by
plasticity. These rounded nanograins can easily roll and rearrange to fill
scratches, and such granular flow is also a form of ductility, although not
of plasticity. (3) The nanograin layer is reminiscent of tribofilms obtained
in industry and rock shear experiments, where sintering (a thermally acti-
vated, diffusion-dominated, plastic process) was claimed as the mecha-
nism forming hard, glossy, wear-protective surfaces (Adachi and Kato,
2000; Hirose et al., 2012).
Connection Between FMs and Seismic Slip
The specific conditions for the formation of our observed FMs are
not known, yet there are two reasons to suspect that slip along them has
been seismic: (1) they are all within the seismically active Dead Sea
transform that separates the Arabian and Sinai plates, and has undergone
more than 100 km of sinistral offset since the Miocene (see Fig. DR1;
Garfunkel et al., 1981); (2) recent experiments suggest that FMs form
only during high shear rates, ~0.15 m/s in sandstones (Hirose et al.,
2012), and ≥0.1 m/s in carbonate gouge (Smith et al., 2013). The for-
mation of FMs was also observed in these experiments to coincide with
strong frictional weakening.
The coupling between FM formation and the weakening process is
not well understood, yet valuable clues are provided by the main FMs
components: the thin layer of nanograins and the smooth hard surface
they form. Powder lubrication has been previously invoked to explain low
friction in a sliding nanograin layer (Han et al., 2010; Reches and Lock-
ner, 2010). However, recent studies have indicated that nanograins cause
weakening mostly at high slip rates, coinciding with formation of FMs
(Tisato et al., 2012; Han et al., 2011). Further study of the rheological
behavior of nanograins under variable slip rates and temperatures should
shed additional light on the formation mechanisms of FMs and their fric-
tional behavior.
ACKNOWLEDGMENTS
We dedicate this paper to the late Hagai Ron, who showed us key fault expo-
sures and provided critical discussions; his friendship, knowledge, and generosity are
greatly missed. We thank C. Scholz, Z. Reches, F. Renard, R. Toussaint, I. Popov,
E. Sharon, and M. Beyth. This work was funded by the Israel Science Foundation and
the James S. McDonnell Foundation. We thank reviewers R. Han and N. De Paola.
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Manuscript received 1 October 2012
Revised manuscript received 25 January 2013
Manuscript accepted 26 January 2013
Printed in USA
www.gsapubs.org | June 2013 | GEOLOGY