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Journal of Archaeological Science: Reports 35 (2021) 102755
Journal of Archaeological Science: Reports
Studies of ancient pottery fragments from Dobrudja region of Romania
using neutron diffraction, tomography and Raman spectroscopy
BA Abdurakhimov a,b M. Belozerova ,
SE Kichanov a,*
a a,d Belc
, M. Bÿlÿÿoiu ,
a
FLNP, Joint Institute for Nuclear Research, 141980, Dubna, Russia
b
Institute of Nuclear Physics, Academy of Sciences of Uzbekistan, Tashkent, 100214, Uzbekistan Museum of
c
National History and Archaeology, 900745, Constant¸a, Romania “Horia Hulubei” National Institute of Physics
d
and Nuclear Engineering, P.O. BOX MG-6, Bucharest-Magurele, Romania Ovidius University, Faculty of Applied Sciences and
It is
Engineering, 900470, Constant¸a, Romania
ARTICLE INFO
Keywords:
Optical microscopy
Neutron scattering methods
Neutron tomography
Raman spectroscopy
Ancient pottery
Ancient Roman ceramics
1. Introduction
The actively developed broad direction in the archaeometry (Jans
sens, 2004; Kardjilov and Festa, 2017; Middleton and Tum, 2006) is
relived by comprehensive studies of cultural heritage objects using
methods of non-destructive testing, such as x-ray and neutron tomog
raphy (Janssens, 2004; Kardjilov and Festa, 2017; Mannes et al., 2015;
Middleton and Tum, 2006), neutron activation analysis (Hughes, 2007)
and others. The obtained results have a unique value because they open
a novel scientific direction to penetrate to the civilizations past, the
evolution of nationalities and historical communities. The uniqueness and
value of museum archaeological items as the cultural heritage ob jects
require modern experimental approaches in their study (Gorgoni et al.,
2002; Kardjilov and Festa, 2017). Recently, more and more attention was
paid to the neutron scattering methods applied in the research of cultural
heritage items (Janssens, 2004; Kardjilov and Festa, 2017; Lehmann et
al., 2007; Mannes et al., 2015; Middleton and Tum, 2006). Neutron
scattering and radiography methods open new up op portunities for the
non-destructive structural diagnostics with high penetration inside the
volume of massive objects (Lehmann et al., 2007;
* Corresponding author at: 141980, Joliot-Curie str., 6, Dubna, Moscow reg., Russia.
E-mail address: ekich@nf.jinr.ru (SE Kichanov).
https://doi.org/10.1016/j.jasrep.2020.102755
Received 19 June 2020; Received in revised form 23 November 2020; Accepted 19 December 2020
2352-409X/© 2020 Elsevier Ltd. All rights reserved.
Contents lists available at ScienceDirect
journal homepage: www.elsevier.com/locate/jasrep
, C. Talmat¸chi M.C.
c
,
D.P. Kozlenko
a
, G. Talmat¸chi
c
,
N.
It is
ABSTRACT
The phase composition and internal structure of several fragments of ancient ceramic amphorae discovered in
archeological excavations in the Dobrudja region, Romania, have been studied using optical microscopy, neutron
diffraction and tomography, and Raman spectroscopy. The good neutron radiography contrast between the
constituent elements of the studied fragments, as well as the high penetration capability of neutron methods,
allow performing non-destructive studies of such archeological items. The bulk phase composition of the am
phora fragments and the spatial arrangement of the main components were determined. The nonuniform dis
tribution of the clay and silicates phases was observed, the volume calculations of presumed silicates grains
were done. The observed structural features of the studied ancient pottery fragments are explained within the
assumption of different chemical processes, that took place during the firing of pottery.
Strobl et al., 2009). The fundamental features of neutron interactions with
matter determine a high penetration ability, sensitivity to hydrogen-
containing materials, good neutron contrast between the neighboring
elements (Banhart, 2008; Kardjilov et al., 2006; Strobl et al., 2009). All
these features make neutron methods valuable for archeological science
research (Janssens, 2004; Kardjilov and Festa, 2017; Kardjilov et al.,
2006; Mannes et al., 2015; Middleton and Tum, 2006).
Multiple fragmentary finds or entirely preserved pottery artifacts make
them objects of great attention of scientists as an extremely important
source of information about the cultural groups and their historical
localization (Bennington, 2004; Moraru and Szendrei, 2011).
Despite the availability and spread of pottery fragments, it should be
noted that ceramics is a complex material with puzzled phase compo
sitions, including several crystalline and amorphous phases (Moraru and
Szendrei, 2011), heterogeneity in the spatial distribution of components
(Stanojev Pereira et al., 2013), doubt concerning the matter of glaze and
pigments of the decoration layers (Papadopoulou et al., 2007), etc.
Knowledge of the pottery composition or clay materials along with surface
decoration patterns can provide novel assumptions about the
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BA Abdurakhimov et al.
manufacturing technology in certain historical periods, the cultural origin
of the artifacts, the internal bulk degradation over time. Sys tematic
studies of ancient ceramics provide interesting historical data including
artistic techniques employed in their decoration, a historical
reconstruction of trade pathways, cultural and social evolution, etc. On
the other hand, non-destructive methods provide structural data like
phase composition, an assembly of hidden components, a spatial
arrangement of cracks and defects, propagation traces of corrosion
(Kockelmann et al., 2000; Moraru and Szendrei, 2011).
In this paper, we report the preliminary results for several model
cultural heritage items, namely some ceramic fragments excavated
during the archeological works in the Dobrudja region, that occupies
the territories between the Danube and the Black Sea (Bocharov et al.,
2017). The ceramic fragments were discovered in the archeological
works at Capidava fortress, close to Constanÿa city, Romania. The
fortress was built during the Roman period at the beginning of the
second century as a castellum, a fundament rebuilt in the second half
of the third century, as part of the system of fortifications protected the
Danube limes (Opriÿ, 2003). It is one of the well-preserved Roman and
Byzantine fortifications in Dobrudja. The position of this fortress near a
ford crossing the Danube has brought it many times to the attention of
migrant populations. Its destruction was inflicted by the Avar-Slavic
attacks on the province of Scythia. The military function of the fortress
was be preserved until the beginning of the reign of Heraclius, later the
fortress regaining its role of protector of the limes towards the end of
the 10th century CE, when it will be rebuilt by the Byzantine
administration (Opriÿ and Raÿiu, 2017; Paraschiv-Talmaÿchi, 2016).
In the present work, the internal structural features of the pottery
fragments have been studied by neutron diffraction and tomography
methods, supported by conventional optical microscopy and Raman
spectroscopy. From a wide variety of ceramic fragments resulting from
the archaeological excavations of the Dobrudja region, we selected
several large fragments of amphora handles, as the model objects, to
demonstrate the opportunities of the neutron methods. The studied
pottery fragments come from transport and table amphorae produced
in Pontic workshops. These types of amphorae were used from the 4th
century until the first half of the 7th century CE (Opaiÿ, 1996; Paraschiv,
2006; Topoleanu, 2000). The pottery artifacts were derived from the
room of a Byzantine edifice used as a storage place located in the
eastern part of the fortress. These were discovered at the destructed
level of the building dated in the second half of the 6th century CE
(Covacef
ˆ andmethods
Potarniche, 2011).ceramic
to identify Along with classical
samples, the archaeological
obtained
structural data can be used for determining the places of manufacture
for the ceramics objects.
Fig. 1. Photos of the investigated pottery fragments. The yellow arrows mark whitish grain-like inclusions in Sample Nÿ2. A scale bar is shown.
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Journal of Archaeological Science: Reports 35 (2021) 102755
2. Materials and methods
For our studies, we have chosen three representatives of archaeo
logical pottery fragments: two that come from types of table amphorae
(Sample Nÿ1 and Sample Nÿ2) and one from a transport amphora
(Sample Nÿ3). In Dobrudja, small table amphorae used for storing or
transporting products over short distances were mainly used to store
and transport the locally produced wine for the garrisons stationed in
the cities (Opaiÿ, 1996). They are considered goods of the provincial
west pontic workshops (type Opaiÿ I), probably from Dobrudja, some
speci mens having a twisted handle and a surface covered with red-
brown or gray-black patterns (Opriÿ, 2003; Topoleanu, 2000). Sample
Nÿ3 comes from an amphora for goods transportation over longer
distances (type Kuzmanov XV). This type of ceramics occurs in the
settlements of the province of Scythia and other western Pontic
territories, but also the northern and north-western Pontic cities (Opaiÿ, 1996; Para
It is believed that these amphorae were produced in workshops of Scy
thia and Moesia Secunda, probably one located in Iatrus (Paraschiv,
2006; Opriÿ, 2003). All amphorae were wheel-thrown.
Photos of the studied ceramic fragments are shown in Fig. 1. The
fragments of curved cylindrical shapes have similar diameters of
approximately 25 mm and lengths close to ~80 mm. All fragments have
a red-brown color. One fragment has a cavern with the remains of am
phora’s body. The fragment Sample Nÿ2 has a distinct spiral pattern on
the surface and some whitish grain-like inclusions (Fig. 1).
Microscopic images of the surface of the pottery fragments were
obtained using a Leica M165 microscope. Raman spectroscopy experi
ments were performed using a spectrometer LabRAM HR (Horiba Gr,
France). The He–Ne laser emits light with the wavelength of 633 nm.
After the scanning procedure, Raman spectra were collected from
several local areas of the pottery fragments. The typical times of spectra
acquisition varied from 5 to 15 min.
To get a comprehensive image of the studied archaeological finds,
it seems justified to use several complementary experimental methods
that provide structural data related to a scale range from crystalline to
micron size (Kardjilov and Festa, 2017; Kichanov et al., 2019).
The phase analysis of the bulk fragments was performed using the
DN-12 neutron diffractometer (Aksenov et al., 1999) located at the IBR
2 high-flux pulsed reactor (Joint Institute for Nuclear Research, Dubna,
Russia). The neutron diffraction spectra were obtained at the scattering
angle of 2ÿ = 90ÿ. The neutron diffraction patterns were fitted by the
profile matching mode using the Fullprof software (Rodríguez-Carvajal,
1993). The exposure time was 20 min.
The neutron tomography data were obtained using the neutron
radiography and tomography facility (Kozlenko et al., 2016, 2015)
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BA Abdurakhimov et al.
located at the IBR-2 high-flux pulsed reactor. The neutron radiography data
has been collected by the scintillator-based detector system with the special
high-resolution CCD camera. The rotation step of the goni ometer in the
tomography experiments was 0.5ÿ. 360 neutron radio graphic images for the
different angular position of the sample relative to the neutron beam direction
was used for the tomography recon struction procedure (Kardjilov et al.,
2011; Lehmann and Kaestner, 2009). The reconstruction of three-dimension
(3D) data of the studied fragments was performed by the SYRMEP Tomo
Project application (Brun et al., 2017). The collection time for one radiography
projection was 20 s. The imaging data were corrected by the dark current
image and normalized to the image of the incident neutron beam using the
ImageJ software (Schneider et al., 2012). Finally, a data set of the vol ume
distribution of 3D voxels was obtained. The dimension of one voxel
is 52 × 52 × 52 µm3 . The 3D volume data of voxels are coded to the bulk
spatial distribution of the neutron attenuation coefficients. The scat tering and
absorption losses form the attenuation of the neutron beam inside the material
(Lehmann and Kaestner, 2009). The visualization and analysis of reconstructed
3D models were performed using VGStu dio MAX software (Volume Graphics,
Heidelberg, Germany).
3. Results
3.1. Optical microscopy
The microscopic patterns of the distribution of components on the
surfaces of the ceramic fragments have been studied using conventional
Fig. 2. Several examples of the optical microscopy images for the studied ceramic fragments. The images were obtained from different local points of the surface of
samples. The scale bars and magnification level of the microscope were shown.
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Journal of Archaeological Science: Reports 35 (2021) 102755
optical microscopy. Selected microscopic images of different points of ceramic
fragments are presented in Fig. 2.
All samples are characterized by a gray-brown clay matrix with well
distinguishable inclusions. In the case of Sample 1, these are small grains of
quartz. However, on the side surface of the ceramic fragment, quite large
grains with sizes up to 500–600 µm are visible. On the side slice of the
ceramic handle, there is a gray core surrounded by a red-brown layer. We
think that this appearance is due to an incomplete firing process during
ceramic manufacturing (Ionescu et al., 2007), which led to oxidative-reductive
ˆ
conditions (Ghergari and Stancel, 2012; Ion et al., 2010). Sample
characterized
2 is by
a more or less uniform distribution of fairly large grains of sand or quartz with
an average size of 100–200 µm. On the surface and the section of the
fragment, large caverns or clumps of sand grains with the average size 500–
600 µm are observed, what looks like poorly sown or coarse sand or sand
clots. We believe that these grains might be remains of calcite, limestone, or
silicates with high birefringence (Emami et al., 2016; Ghergari and Stancel,
ˆ
2012). Besides, on the surface of these large grains, there is Several
a white coating.
cracks
and cavities on Sample 2 surface are visible.
The surface of Sample 3 is represented by a mixture of light and dark red-
brown areas. There are several deep caverns and light calcite in clusions on
the surface.
3.2. Raman spectroscopy
The Raman spectra obtained from selected points of the pottery fragments
surfaces are shown in Fig. 2. The most intense Raman lines at
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BA Abdurakhimov et al. Journal of Archaeological Science: Reports 35 (2021) 102755

1161, 808, 463, 356, 265, 207, and 128 cmÿ quartz phase 1 can be related to the
(Germinario et al., 2018; Medeghini et al., 2014; Mernagh, 1991). The weak peaks at 510
1
and 394 cmÿ can correspond to the feldspar and hematite phase,
position
respectively.
indicates aThe
possible
peak
predominance of the silicate mineral of the labradorite ((Ca, Na)(Al, Si)4O8) in the feldspar
phase (Mernagh, 1991). On one of the Raman spectra (not shown here), a strong line at
3189 cmÿ of stretching vibrations ÿ(O–H) was observed, which may indicate the presence
1
of a local amount of water or some hydroxides.

3.3. Neutron diffraction

The neutron diffraction spectra of the studied pottery fragments are shown in Fig. 3.
A rather complex background of neutron patterns in dicates the amorphous phase of clay
(Kockelmann et al., 2001). The observed diffraction peaks have corresponded to the
quartz phase (Ghergari and Stancel, 2012; Kockelmann et al., 2001). The crystal
ˆ
structure of this phase is described
4.908(5)
by P3121
Å andspace
c = 5.414(4)
group with
Å. There
unit cell
are parameters
some addi tional
a=
diffraction peaks on the neutron pattern of Sample 1. We think that these diffraction peaks Fig. 4. Neutron diffraction spectra of the pottery fragments. The experimental
correspond to an additional phase of orthoclase (Ghergari and Stˆ ancel, 2012; Ionescu points and fitted profile are shown. Ticks are calculated positions of the Bragg
et al., 2007). The crystal structure of this phase is described by monoclinic C12/ m1 sym peaks of quartz and orthoclase phases. The diffraction peaks of the orthoclase
metry with lattice parameters a = 8.622(9) Å, b = 12.997(6) Å, c = 7.222(8) Å, and ÿ = phase are marked.
116.5(1)o .
volume comprises 107,800 voxels or 15.2 mm3 of the ,
while the entire volume
Sample 1 fragment consists of 47,859,248 voxels or 6729 mm3 The calculated volume .

fraction of the silicates components in the studied fragment is 0.2%. The average volume
of the silicates grains is 0.08 mm3 The 3D model of Sample 2 after tomographic
reconstruction
but the is shownvalue
median in Fig. 6. Themm3
is 0.012 large presumably silicate grains with high neutron
3.4. Neutron tomography
.
,

The spatial distribution of the internal components of the pottery fragments was
studied using the neutron tomography method. The dif ferences in the composition of
various components in the studied ceramic fragments led to the neutron radiographic
contrast.
The reconstructed 3D model of the pottery Sample 1 is presented in Fig. 5. It is
observed that neutron absorption inside the pottery fragment volume is nonuniform.
Several near-surface areas attributed to regions with higher neutron attenuation coefficient
are visible. We suggest that differences in the neutron absorption are related to the
incomplete firing process during amphora manufacturing (Ghergari and Stˆ ancel, 2012;
beam attenuation coefficients, as well as large and small cavities and cracks were
observed. It should be noted that at the base of the handle there are
a large number of elongated cracks and caverns (Fig. 6), that may indicate the layered
structure of the amphora handle, which was often noted in other studies (Bocharov et al.,
2017; Emami et al., 2016).
Several morphological futures for detected silicate grains were ob tained. These
grains occupy about ~0.9% of the total pottery fragment volume. The sizes of the
shapeless grains were analyzed in terms of an equivalent diameter (Gregorova et al.,
´

Ion et al., 2010; Ionescu et al., 2007), which is a reason for different degrees of oxidation 2009). The obtained distributions of the equivalent
Sample 1 and
diameters
2 are presented
of the silicate
in Fig.
grains
7. The
for
in the core and surface regions. In addition to the surface layers, several rounded characteristic sizes of the most silicate grains fall into the range of 0.2–1 mm, the larger
formations are observed in the volume of the pottery Sample 1 (Fig. 4), which might be diameter is 2.76(2) mm. Among the differences, we should note the more isotropic
grains of the orthoclase phase or other silicates (Ghergari and Stancel, 2012). Those distribution of the neutron attenuation coefficient over the entire volume of Sample 2. The
grains near-surface layer observed in Sample 1 was not detected. It can be assumed that this
ˆ fragment of amphora had different firing conditions, but to confirm this hypothesis, more
detailed physical and chemical studies are required.

The reconstructed 3D model of the pottery Sample 3 is shown in Fig. 8. Surprisingly,

there are no silicate grains detected in this sample.
An uneven surface layer up to 2–3 mm thickness as in Sample 3 was found. The
.A
calculated volume occupied by this layer was 30.2(3) mm3 large number of spherical voids
are visible in the volume of Sample 3 fragment.

It can be seen that the first two fragments of ceramics are charac terized by the
presence of large grains of quartz and orthosilicates. In Sample 1, there is a strong effect
of spatial phase separation due to a violation of insufficient firing technology. Although a
decorative spiral pattern is visible on Sample 2, a roughness of the ceramic processing
can be explained by the lower and cheaper technological requirements for the amphorae
used to carry and store wine for the soldiers of the ancient fortress garrison (Opaiÿ, 1996).
In contrast, there are no large coarse silicate grains in the amphora of Sample 3. Here,
we should take into account the different locations of the pottery workshops, as well as
more demanding rules in the production of amphorae for long-term trans portation of a
product. As a final remark, it should be noted that our

Fig. 3. Raman spectra obtained from selected areas on the surface of the pot
tery fragments Sample 1, 2 and 3. The corresponded Raman lines of dominant
phases are labeled: quartz (Qtz), feldspar (F) and hematite (Hem).

4
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BA Abdurakhimov et al. Journal of Archaeological Science: Reports 35 (2021) 102755

Fig. 5. The 3D model after tomographic reconstruction, longitudinal and transversal slices of the 3D model of the pottery fragment Sample 1. The rainbow-like
coloring shows a neutron absorption degree from low (blue) to high (red). The regions with lower neutron attenuation coefficient can be attributed to areas with
the incomplete firing process. A scale bar is shown.

Fig. 6. The 3D model after tomographic reconstruction, longitudinal and transversal virtual slices of the 3D model of the pottery fragment Sample 2. The rainbow
like coloring shows neutron absorption degree from low (green) to high (red). The high attenuation coefficient of neutron can be attributed to the silicates grains
inside the volume of the fragment. A scale bar is shown.

Fig. 7. The distribution of the equivalent diameters of the observed silicate grains inside the ancient pottery Sample 1 and 2.

5
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BA Abdurakhimov et al.
Fig. 8. The 3D model after tomographic reconstruction, longitudinal and transversal virtual slices of the 3D model of the pottery fragment Sample 3. The rainbow
like coloring shows neutron absorption degree from low (green) to high (red). The regions with lower neutron attenuation coefficient can be attributed to areas with
incomplete firing process. The dark-blue rounded holes are hidden voids and cracks inside bulk of the fragment. A scale bar is shown.
primary results can open new scientific directions of analysis based on
structural characteristics for the identification of ceramic samples,
complementing the existing ones.
4. Conclusions
Our research demonstrates the utility of the neutron methods like
tomography and diffraction, which can be used as complementary sci entific
tools for the characterization of the pottery finds. These methods can be
employed in combination with classical analytical methods, such as
petrography and electron microscopy that are traditionally employed in the
characterization of pottery artifacts.
In this paper the results of a study on the bulk structure of several
representatives for the ancient pottery found on the territory of the Dobrudja
region, Romania is reported. The fragments of amphorae were probed by
neutron methods, such as neutron diffraction and tomogra phy, supplemented
by Raman spectroscopy and optical microscopy.
These results provide a good illustration of the possibilities of neutron
methods as a non-destructive structural diagnostic tool for archaeolog ical
ceramics samples. The high penetrating feature and the nature of the
interaction of neutrons with matter allowed the non-destructive deter
mination of the crystalline phase composition of the volume of the pottery
fragments, as well as to clarify some structural features of these archeological
items. The differences in the neutron attenuation co efficients of the
constituent elements of the studied ancient pottery fragments allowed
obtaining the spatial distribution of different phases inside of the volume of
these amphora handles. Using neutron tomog raphy, some rather large
grains of presumable silicates were found in the volume of Sample 1 and
Sample 2 pottery fragments. The size distri bution of those silicate grains was
obtained. The obtained structural features can be used to identify the place
of origin of the ancient ceramic products. Also, for Samples 1 and 3, a near-
surface layer with a high neutron attenuation coefficient was detected. Due
to the sensitivity of neutron methods for the concentration of various oxides,
the formation
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Journal of Archaeological Science: Reports 35 (2021) 102755
of these layers can be explained by the oxidation processes during the firing
of ceramics or chemical processes, while preserving the integrity of the
studied archaeological ceramic items. The integrated approach used in this
pilot study offers a perspective for the study of archaeo logical objects,
offering new insights about the bulk structure of the investigated finds and
offering information about the techniques employed in the manufacturing of
ancient pottery.
Funding
This research did not receive any specific grant from funding
agencies in the public, commercial, or not-for-profit sectors.
CRediT authorship contribution statement
B.A. Abdurakhimov: Methodology, Software, Validation, Formal analysis,
Investigation, Writing - original draft, Visualization. S.E.
Kichanov: Conceptualization, Methodology, Validation, Investigation, Writing
- original draft, Visualization. C. Talmat¸chi: Conceptualization, Writing -
original draft. D.P. Kozlenko: Software, Validation, Supervi sion, Funding
acquisition. G. Talmat¸chi: Resources, Project adminis tration, Funding
acquisition. N.M. Belozerova: Methodology, Formal analysis, Investigation.
M. Balasoiu: Project administration, Funding acquisition. M.C. Belc:
Validation, Resources, Supervision, Project administration, Funding
acquisition.
Conflicts of Interest
The authors declare no conflict of interest.
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