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Orientalizing Artifacts from Fraga dos Corvos
Rock Shelter in North Portugal
Article in Materials and Manufacturing Processes · September 2009
DOI: 10.1080/10426910902982508
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Orientalizing Artifacts from Fraga dos Corvos Rock Shelter in North Portugal
E. Figueiredo abc; J. C. Senna-Martinez d; R. J. C. Silva c; M. F. Araújo a
Instituto Tecnológico e Nuclear (ITN), Sacavém, Portugal b Departamento de Conservação e Restauro,
Faculdade de Ciências e Tecnologia, Universidade Nova de Lisboa, Monte de Caparica, Portugal c Centro de
Investigação de Materiais (CENIMAT/I3N), Faculdade de Ciências e Tecnologia, Universidade Nova de
Lisboa, Monte de Caparica, Portugal d Centro de Arqueologia (Uniarq), Faculdade de Letras, Universidade de
Lisboa, Lisboa, Portugal
a
Online Publication Date: 01 September 2009
To cite this Article Figueiredo, E., Senna-Martinez, J. C., Silva, R. J. C. and Araújo, M. F.(2009)'Orientalizing Artifacts from Fraga dos
Corvos Rock Shelter in North Portugal',Materials and Manufacturing Processes,24:9,949 — 954
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Materials and Manufacturing Processes, 24: 949–954, 2009
Copyright © Taylor & Francis Group, LLC
ISSN: 1042-6914 print/1532-2475 online
DOI: 10.1080/10426910902982508
Orientalizing Artifacts from Fraga dos Corvos Rock Shelter
in North Portugal
E. Figueiredo123 , J. C. Senna-Martinez4 , R. J. C. Silva3 , and M. F. Araújo1
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2
1
Instituto Tecnológico e Nuclear (ITN), Sacavém, Portugal
Departamento de Conservação e Restauro, Faculdade de Ciências e Tecnologia, Universidade Nova de Lisboa,
Monte de Caparica, Portugal
3
Centro de Investigação de Materiais (CENIMAT/I3N), Faculdade de Ciências e Tecnologia,
Universidade Nova de Lisboa, Monte de Caparica, Portugal
4
Centro de Arqueologia (Uniarq), Faculdade de Letras, Universidade de Lisboa, Lisboa, Portugal
An unusual set of metallic artifacts with orientalizing character, attributed to a late period of the Late Bronze Age (LBA), was found in a shelter
in Northern Portugal. Conventional and micro-energy dispersive X-ray fluorescence (XRF) analyses have been performed to determine the metal
composition. The microstructures of some artifacts have also been studied under optical and scanning electron microscope (SEM). The results
show that most of the items are made of a copper–tin alloy with low lead content and show a recrystallized grained microstructure.
Keywords Archaeometallurgy; Bronze; Iberian Peninsula; Late Bronze Age; Microstructure.
presence of Phoenicians on the Iberian coasts, are much
scarcer than those on the earlier Atlantic tradition.
Analyses of metallic items from the Phoenician site of
Almaraz (on the western coast of Portugal) determined
alloys with low Sn and variable Pb contents [7], which can
be easily distinguished from the previous alloys used during
the LBA.
Analyses of numerous metallic items from the
orientalizing site of Cancho Roano (southwest of Spain,
dated to the middle of the first millennium B.C.)
showed erratic alloy compositions, with highly variable
concentrations of Sn and Pb [8].
More recent studies, concerning orientalizing sites dated
to the 7–6th century B.C., as El Palomar and Medellín
(Extremadura, Spain), determined Cu–Sn alloys with
percentages and impurity patterns quite different from those
of Cancho Roano (which has a later chronology). In both
sites, the majority of the items were of bronze with <2%
Pb; a small number of bronze with a high amount of Pb
(mainly large sized objects); and a few pieces were made
of unalloyed copper [9].
During the archaeological excavations in a rock shelter at
Fraga dos Corvos site (Macedo de Cavaleiros) in northern
Portugal, a number of metallic items of orientalizing type
were found. The group of artifacts comprises a double
resort fibula, two needles, a flat pendant, decorated on
both sides with dotted lines which form star-shaped motifs,
and a cosmetic spatula. Further eight bar-shaped fragments
(comprising possibly fragments of a bracelet and a ring)
and one metallic nodule were found (Fig. 2).
Typologically, the group of artifacts has a Mediterranean
character which suggests a Phoenician origin or, at least,
a strong influence from the southern areas of the Iberian
Peninsula. Additionally, the decoration of the pendant finds
1. Introduction
Studies on Late Bronze Age (LBA) metal artifacts (dated
between the end of the 2nd millennium to the early 1st
millennium B.C.) showed that the bronze composition used
in the Iberian Peninsula contains Pb as a minor constituent,
with percentages regularly <1%. This is significantly
distinct from the alloy used in other “Atlantic” areas,
such as the English and French territories, where the Pb
content can regularly reach values up to 10% [1]. All
artifacts from Ria de Huelva, southern Spain, and those from
central Portuguese sites, such as Santa Luzia, Canedotes,
Sernancelhe, Monte do Frade, Alegrios, and Moreirinha
[2–5] show tin values between 8–14%, and no or very
low Pb (Fig. 1). This metal type shows more similarities
with that of Mediterranean areas. However, the bronze
employed in the rest of the Mediterranean in the LBA (or, in
the contemporary Eastern Mediterranean, in the Iron Age),
shows regularly a lower Sn content (7–9% or less) and
commonly a Pb content of 1–3% [1, 6].
Higher variations in Sn content and higher Pb content
only became common in the artifacts of the Iberian
Peninsula at the beginning of the Iron Age. The transition
from Bronze to Iron Age happens, at least in the south of the
Iberian Peninsula, with the beginning of the Orientalizing
period. In the Northern Iberian regions, the Orientalizing
influences are not as evident as in the south; therefore,
the LBA continues here until the mid-first millennium.
The studies on Orientalizing metal artifacts, related to the
Received January 10, 2008; Accepted November 30, 2008
Address correspondence to E. Figueiredo, Instituto Tecnológico e
Nuclear, Estrada Nacional 10, 2686-953 Sacavém, Portugal; Fax: +351219946185; E-mail: elin@itn.pt
949
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950
Figure 1.—Location of the mentioned archaeological sites in which artifacts
show strong Atlantic typological features (white dots) and orientalizing
typological features (black dots) in the Iberian Peninsula.
close parallels in the orientalizing graffiti on the grey ware
of Medellín [10].
The items were found in disturbed layers; however, the
typology of the objects suggests that they are part of one
set of artifacts, probably of a funerary deposit belonging to
a late period of the LBA [11].
Experimental
All items were at first, without surface preparation,
submitted to energy dispersive X-ray fluorescence (EDXRF)
analyses to identify the type of alloy(s). These results were
Figure 2.—Image of some of the artifacts found in Fraga dos Corvos shelter.
From left to right, top to bottom: pendant FC-215; needle FC-188; fibula
FC-181; nodule FC-474; Tartessian belt hook fragment FC-473; and cosmetic
spatula FC-361.
E. FIGUEIREDO ET AL.
interpreted as semiquantitative, because of the presence of
superficial corroded layers. Indeed, several phenomena may
induce changes on the overall composition of the exposed
area of the artifacts, i.e., superficial decuprification which
leads to enhanced concentrations of the other alloy elements
[4] or enrichment of other elements in soil (i.e., Fe) easily
incorporated in corrosion layers.
The EDXRF analyses were carried out in a Kevex
771 spectrometer, with secondary targets that allow
the optimization of the analytical conditions. Certified
reference materials phosphor bronzes from the Burial of
Analysed Samples LTD and leaded bronzes from the
BNF Metals Technology Centre were used to calibrate the
spectrometer. Detailed description of the equipment [12],
and quantification procedures were described elsewhere
[3, 4].
Subsequently, small samples were taken for
metallographic examination from three bar fragments,
the ring(?) fragment, a bracelet(?) fragment and from
the metallic nodule. All samples were mounted in cold
mounting epoxide resin and polished with SiC abrasive
paper and diamond suspension (up to 1/4 m) following
the usual procedure.
On three more artifacts (needle FC-457, cosmetic spatula
FC-361, and tartessian belt hook fragment FC-473) a small
area of the surface was cleaned from superficial corrosion
and polished (without sampling). All items were examined
by optical microscope (OM) in bright field (bf), polarized
light (pol), and dark field (df), both in unetched and etched
conditions. The etching was carried out by using an aqueous
ferric chloride solution.
Micro-EDXRF analyses were also conducted on all
cleaned and polished areas, for the elemental determination
of the alloy composition. These analyses were performed
by using an ArtTAX Pro spectrometer, with a low-power
X-ray tube with a molybdenum anode, and a set of
polycapillary lenses generating a microspot, lower than
100 m in diameter, of primary radiation.
The quantification analyses were carried out by using
WinAxil software. The calibration was done by using
the same reference materials employed for EDXRF. The
quantification procedures were recently described [3, 4].
Additionally, micro-EDXRF analyses were also
conducted on two artifacts (the needle FC-188 and the
fibula FC-181) on an area with a recent fracture, and
therefore, free of superficial corrosion layers.
A selected sample (FC-206 bar fragment) was also
observed under SEM, model Zeiss DSM 962, with
secondary electron detector (SE), backscattered electrons
detector (BSE), and energy dispersive spectrometer (EDS)
from Oxford Instruments model INCAx-sight with an
ultrathin window. The analyses and examinations carried
out on the artifacts are listed in Table 1.
Results and Discussion
The EDXRF analyses allowed the identification of the
alloy employed for the artifacts: all items, with exception
of the Tartessian belt hook fragment FC-473 which is made
of copper with Sn and Pb as minor elements, were made of
bronze (Cu–Sn), in most cases with some Pb.
951
ARTIFACTS FROM FRAGA DOS CORVOS
Table 1.—Analyses of studied metal artifacts.
EDXRF
Pendant FC-215
Fibulae FC-181
Needle FC-188
Needle FC-457
Cosmetic spatula FC-361
Bar frag. FC-215
Bar frag. FC-206
Bar frag. FC-208
Ring(?) frag. FC-120
Bracelet(?) frag. FC-364
Bracelet(?) frag. FC-362
Tartessian belt hook frag. FC-473
Metal plate FC-475
Nodule FC-474
∗
×
×
×
×
×
×
×
×
×
×
×
×
×
×
Micro-EDXRF
OM
×∗∗
×∗∗
×∗
×∗
×∗
×∗
×∗
×∗
×
×
×
×
×
×
×∗
×∗
×
×
×∗
×
SEM-EDS
×
On the area prepared for metallographic examination.
On a recent fracture surface.
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∗∗
The metallic nodule FC-474 is the only object which
shows a Pb content higher than the Sn content (Table 2).
The micro-EDXRF results allowed the assessment of the
metal composition. The ten items analyzed can be grouped
in a region with 8–13% Sn and Pb <2%, and can thus be
considered binary bronze alloys (Fig. 3).
The needle FC-457 seems to have a highly heterogeneous
Pb distribution (cf. high standard deviation), probably
related to the strong intergranular corrosion in the area
analyzed (see below metallographic examination), which
did not allow to determine the Pb content with accuracy.
The higher standard deviation determined for the tin
contents in FC-188 and FC-181 are probably also related
to some internal corrosion, as the micro-EDXRF analyses
were done on fractures (Table 1). As the EDXRF analyses
suggest, the metallic nodule FC-474, is made of a different
alloy. A higher Pb and a lower Sn content distinguish it
from all other bronzes.
The Tartessian belt hook fragment FC-473, is made of
copper with tin and lead as minor elements, and can be
considered unalloyed copper.
The cluster of the seven items (8–13% Sn and <2% Pb)
represents an alloy with 101 ± 15% Sn and 11 ± 06%
Pb which can be considered a good quality bronze, with
values that do not depart much (possibly a slightly higher
Pb content) from the metallurgical tradition of the Iberian
Bronze Age. However, the metallic nodule shows a different
composition, with ∼5.5% Sn and 6% Pb. These are not
common Sn and Pb values for LBA artifacts of the Iberian
Peninsula.
The artifacts ensamble has perhaps parallels in the
artifacts represented on LBA/Early Iron Age warrior stelae
(distributed through the referenced areas). The stelae show
figures of (possibly) warriors with their personal items.
Frequently represented are fibulae, possibly a mirror with
a shape similar to that of the pendant, and small circular
items, similar to metallic nodules.
Considering the complete set of artifacts, the
compositions show the strongest resemblance with the
bronzes from El Palomar and Medellín. Also the typological
features of the artifacts from Fraga dos Corvos find close
matches among the objects from El Palomar and Medellín.
Metallographic examinations revealed that all items,
with the exception of the metallic nodule (FC-474), have
recrystallized -grains (twinned) and absence of +
Table 2.—Results of EDXRF (a) and micro-EDXRF (b) analyses (n, number of analyses performed on each artifact).
Pendant FC-252
Fibulae FC-181
Needle FC-188
Needle FC-457
Cosmetic spatula FC-361
Bar frag. FC-215
Bar frag. FC-206
Bar frag. FC-208
Ring(?) frag. FC-120
Bracelet(?) frag. FC-364
Bracelet(?) frag. FC-362
Metal plate FC-475
Tartessian belt hook frag. FC-473
Nodule FC-474
a n = 2
a n = 1
b n = 3
a n = 2
b n = 3
a n = 2
b n = 3
a n = 2
b n = 3
a n = 1
b n = 3
a n = 1
b n = 3
a n = 2
b n = 3
a n = 2
b n = 3
a n = 2
a n = 2
b n = 3
a n = 2
a n = 2
b n = 3
a n = 1
b n = 3
Cu
wt%
Sn
Pb
As
Fe
+++
+++
871 ± 37
++
874 ± 17
++
828 ± 46
++
899 ± 08
++
890 ± 08
+++
892 ± 05
++
886 ± 02
+++
868 ± 03
+++
+++
894 ± 01
++
+++
984 ± 01
++
883 ± 078
++
+
112 ± 39
++
111 ± 15
+
122 ± 08
++
89 ± 09
++
81 ± 02
+
86 ± 05
+++
98 ± 02
++
122 ± 02
++
++
139 ± 59
++
–
08 ± 01
+
55 ± 04
–
–
06 ± 02
+
11 ± 03
+
48 ± 41
+
12 ± 02
+
18 ± 06
+
20 ± 03
+
13 ± 00
–
08 ± 02
n.d.
n.d.
n.d.
+
–
04 ± 01
++
61 ± 07
n.d.
n.d.
<0.1
n.d.
01 ± 00
n.d.
01 ± 00
n.d.
n.d.
n.d.
<0.1
n.d.
n.d.
n.d.
<0.1
n.d.
<0.1
vest.
vest.
n.d.
n.d.
vest.
02 ± 00
n.d.
n.d.
vest.
–
06 ± 01
–
009 ± 003
–
003 ± 001
–
005 ± 001
–
01 ± 01
–
<0.04
–
004 ± 00
–
004 ± 004
–
–
<0.04
–
–
011 ± 003
–
<0.04
n.d. = not detected.
In EDXRF analyses: (vest.) <1%; (–) 1–10%; + 10–30%; ++ 30–50%; + + + > 50%; results with influence from corrosion composition.
Others
vest.
Sb
Sb, Ni
Sb
Sb, Ni
Sb, Ni
Zn
Sb
Zn
Sb
Zn
Sb
Zn
Zn
Ni, Zn
Sb, Ni, Zn
Sb, Ni
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952
E. FIGUEIREDO ET AL.
Figure 3.—Plot of the Sn and Pb mean contents obtained by micro-EDXRF analyses on the metal bulk of the artifacts. Standard deviations higher than 1 are
illustrated.
eutectoid. With normal casting cooling rates, as attained
in sand castings, in bronzes with 8–12% Sn a biphasic
microstructure is expected.
According to the nonequilibrium binary phase diagram
for copper-tin metal alloys, the -copper phase would be
the only phase in the microstructure of an alloy with up to
15% Sn when a homogenizing heat treatment, as annealing,
is performed. This heat treatment will improve the bronze
mechanical properties since it results in the absence of the
brittle phase in the final microstructure. In the case of a
previous mechanical work a posterior heat treatment would
help to recover ductility, by promoting a recrystallization
process.
Final mechanical work can increase/adjust the final
hardness by a strain hardening effect or it may be carried
out for final shape adjustments.
In the examined artifacts, the metalwork consisted in
thermomechanical operations, such as cold-forging (to
obtain the required shape and harden the metal) followed
by annealing (by which the metal became soft again).
On some items, such as bar fragment FC-215, ring
fragment FC-120, bracelet(?) fragment FC-362, and needle
FC-457, strain bands are also observed. They are probably
due to some residual cold work in the final stage of
metalwork (Fig. 4).
Intergranular corrosion is present mainly near the
surfaces. After the superficial polishing of the needle FC457, intergranular corrosion along grain boundaries and
Figure 4.—OM image of ring(?) fragment FC-120 revealing -phase
recrystallized grains (twinned) with strain bands (etched, BF).
Figure 5.—OM image of needle FC-457 with inter- and intragranular
corrosion (unetched, BF).
ARTIFACTS FROM FRAGA DOS CORVOS
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along crystallographic planes (i.e., due to the final cold
work) became visible all over the prepared area (Fig. 5).
All microstructures reveal the presence of pores, in
various number and sizes, as well as the presence of sulphide
inclusions (Cu–S). The presence of sulphide inclusions, just
by itself, does not mean that the ores used in the production
of the metal were copper sulphides. If during reduction
other minerals rich in sulphur were in contact with the
forming metal, sulphur could be incorporated into the metal.
Only posterior refining operations would reduce the sulphur
content, but the examined microstructures do not seem to
indicate that this took place.
Generally, the artifacts with the thinnest sections are
also those with the smallest pores and the most distorted
sulphide inclusions. The FC-206 bar fragment has the
largest cross-section size and is the only item with pores
Figure 6.—BSE image of bar fragment FC-206. EDS analyses have been
performed on: (1) matrix composed by -phase; (2) lead globules; (3) sulphur
inclusions.
953
>100 m. This is also the only fragment with some of
the as-cast microstructure morphology (pseudomorphism).
All lead globules and sulphide inclusions are aligned and
indicate the direction and an estimation of the (secondary)
dendritic arms spacing (DAS ∼23 m) which grew during
the solidification of the alloy (Fig. 6). Posterior forging did
not disturb the alignment.
The FC-474 metallic nodule has an as-cast microstructure
with the formation of dendrites which have an arm
spacing (DAS) of ∼25 m. It shows a small amount of
interdendritic eutectoid, shrinkage cavities, and Pb globular
or interdendritic forms (Fig. 7).
Metallic nodules can be a result of a reducing operation
(transformation from ore to metal), in which they are formed
and trapped among the nonmetallic material, or they can
be a result of the casting (when metal is poured from the
crucible to the mould), if some metal drops out. In the
first case, and in the case of a co-smelting process of Cu
and Sn ores, the resulting nodules would show irregular
compositions (S. Rovira, personal communication). In the
second case, the composition would be similar to the metal
composition of the object(s) produced.
The microstructure can also provide information on the
character of the nodule due to a different solidification
rate: slow solidification rate for a smelting nodule; fast
solidification for a casting nodule. Thus, the microstructure
of a smelting nodule should show dendrites with arm
spacing larger than that of a casting nodule. Depending
on the rate of solidification, and particularly in the second
case, it is also possible that no formation of dendrites takes
place. Furthermore, depending on the Sn concentration, the
formation of the + eutectoid would be favored in
the second case, since the cooling would be far from the
equilibrium conditions.
In the present study, because of the small size of the
metallic nodule, its microstructure does not allow clear
conclusions. However, its distinctive composition (different
from that of all the other analysed items), suggests that it
was produced by smelting.
Figure 7.—OM image of metallic nodule FC-474 showing dendritic structure
(unetched, BF).
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954
E. FIGUEIREDO ET AL.
Conclusions
The stylistic characterisation of the artifacts is supported
by the results of the elemental analyses. The metal
compositions of the items found in Fraga dos Corvos rock
shelter does find close associations with the metallurgical
tradition of the orientalising sites of Medellín and El
Palomar, where the binary bronzes (<2% Pb) are in
the highest proportion, followed by ternary bronzes and
unalloyed copper.
The similarities among the pendant decoration and the
orientalizing graffiti found on Medellín grey ware do not
seem to be casual and apparently confirm the interpretation.
The metallographic observations suggest that the
manufacture of small and simple items, as fibulae,
bracelet(?), ring(?), cosmetic spatula, belt hook, and bar
fragments found in the Fraga dos Corvos hoard, was
carried out by working predefined forms, such as bars cast
previously in a mould, and further worked to final shape
through forging/annealing operations.
Metallographic examinations showed that the annealing
treatment was long enough to homogenize the alloy and
solubilize any remains of the eutectoid phase resulting in
a decrease of brittleness and in an increase of tenacity of
the metal.
The rather plain surfaces and simple shapes could be
decorated, in a final stage, with a pointed chisel, as in the
case of the pendant.
The composition of the metallic nodule suggests that this
item might have been produced during a smelting process.
The presence of this item among other artifacts at the site
also suggests that metal nodules might have been kept and
traded as raw material.
Acknowledgments
This work has been carried out in the framework of the
project POCTI/HAR/58678/2004, Metallurgy and Society
in Central Portugal LBA, financed by the Portuguese
Science Foundation (FCT). The first author acknowledges
the FCT for the SFRH/BD/27358/2006 grant.
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