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1. INTRODUCTION
The firing temperatures of ancient ceramics are of interest because they provide
information on the performance of the kilns used in their manufacture and on
the technological capabilities of the ancient potters. Apart from its immediate
archaeological significance, this information is essential for “experiments” in
which full-scale replicas of excavated pottery kilns are built and fired (Mayes,
1961 and 1962). In addition a knowledge of the firing temperature can be of
value in other scientific investigations of ancient ceramics and kilns, such as
thermoluminescent and magnetic dating.
Two different methods have previously been used in the determination of
the firing temperature of ancient ceramics. In the first, a rough indication of
the firing temperature is obtained through studying the minerals present in the
ceramic by means of X-ray diffraction techniques, optical microscopy and
differential thermal analysis (Tobler 1939, Felts 1942, Mariani et al. 1956, Perinet
1960). In the second, the firing temperature is estimated using the data obtained
from thermal expansion measurements on the ceramic.
The thermal expansion method is based on the assumption that when clays are
fired, shrinkage occurs as a result of various sintering processes (i.e. densification
through agglomeration of the fine clay particles). Consequently if a fired clay
ceramic is heated up steadily from room temperature, it exhibits normal reversible
thermal expansion, characteristic of its mineralogical composition, until tempera-
tures comparable with its original firing temperature are reached. With continued
increase in temperature, the ceramic begins to contract since, superimposed on
the reversible expansion, there is an irreversible shrinkage associated with the
resumption of sintering (i.e. the firing of the ceramic is being continued beyond
the point reached during its original firing). The temperature (T,) at which
expansion ceases and contraction begins should therefore provide an estimate
of the original firing temperature (T& the former being defined as the “shrinkage
temperature”.
In principle this method should, with appropriate corrections, provide a more
precise value for the firing temperature than that based on a “mineralogical
temperature scale”. Reasonably satisfactory results have been obtained by Kiefer
(1956). Terrisse (1959) and Roberts (1963). However Matson (1937), working with
low-fired American Indian pottery, observed an irreversible expansion in the
500-800°C range while Cole and Crook (1962), working with Roman brick,
observed a complicated pattern of irreversible expansion and contraction. As
a result of these discrepancies, a detailed investigation into the assumptions, on
which the thermal expansion method is based, was undertaken in order to
establish its validity and accuracy for the determination of firing temperatures
*Present address : Department of Physics, University of Essex.
132 ARCH AEOMETRY
(Section 3). Subsequently the method was used to provide an estimate of the
firing temperature of a wide selection of ancient ceramics (Section 4).
2. APPARATUS
A fused silica extension rod dilatometer. similar to that described by Roberts
(1963), was used for thermal expansion measurements up to 1000°C. For measure-
ments on ceramics fired at temperatures greater than 1000”C, a dilatometer with
polycrystalline alumina components and based on a design by Raudran (1955),
was employed.
In both cases, the specimen and dilatometer assembly were heated in a
platinum-wound tubular furnace (Johnson Matthey and Company Limited: Type
K45B), the heating rate being 200°C per hour, and the change in length of the
specimen was measured using a variable inductance transducer (Boulton Paul
Aircraft Limited: Type F19). The output of the transducer was fed to the Y axis
of a Honeywell Brown X-Y recorder (Model 153 x 32) and the e.m.f. from the
thermocouple, used to measure the temperature of the specimen, was fed to
the X axis, thus providing a plot of the change in length of the specimen versus
temperature.
Changes in specimen length of 0.2 micron (ix. approximately for a
2.5 cm specimen) could readily be measured with both dilatometers and for a
typical specimen the temperature at which shrinkage began could be estimated
with an accuracy of k 5°C. Further details concerning the construction and
performance of the dilatonieters are presented in reports by Tite and Roberts
(1966 and 1969).
3. PRELIMINARY INVESTIGATIONS
The basic problem, in determining the firing temperature of ancient ceramics
from thermal expansion measurements, is to establish the relationship between
the shrinkage temperature (T,) and the original firing temperature (T,) or
“equivalent firing temperature” (T,J*. This relationship is governed by the
dimensional changes occurring when the clay, used in the manufacture of the
ceramic, is heated and these changes depend critically on the clay minerals
(e.g. kaolinite, montmorillonite and illite) and impurities (e.g. quartz, carbonates,
iron oxides and organic matter) present.
Those mineralogical and dimensional changes, relevant to the determination of
firing temperatures, can be summarised as follows (Kiefer 1952 and 1957, Ford
1967): -
(i) When the clay loses chemically combined hydroxyl water (400-6OO0C), a
contraction occurs in the case of kaolinite and an expansion in the case of
montmorillonite and illite. This contraction or expansion then continues at a
greatly reduced rate until a rapid shrinkage, associated with either vitrification
or the formation of high-temperature phases ( e g spinel, mullite), begins
(figure 1).
* The “equivalent firing temperature” (Teq),estimated from thermal expansion measurements
in the case of ancient ceramics, is essentially that constant temperature which would have
brought about the same amount of sintering as was achieyed during the original firing. The
term, firing temperature (Te), has no precise meaning since it is probably that, with many
ancient ceramics, the technique of heating to a peak temperature, followed by immediate
cooling, would have been employed and therefore a major part of the shrinkage, or
sintering, would have taken place at temperatures below the peak temperature.
ARCHAEOM ETRY 133
"0 500 m -0
T'C T"C
FIG. 1. Thermal expansion curves for unfired and prefired specimens of (a) Farnley Fireclay,
(b) Dorset Ball Clay: percentage change in length (AL) versus temperature (TOC).
TABLE I
Mirterologicul Vitrification Firing
Cloy composition temp. (T."C) temp. (T,"C) (T. - Td"C
Q K M
London Clay s s a 710 768 - 22
948 + 38
Etruria Marl a a s 850 750 - 26
Dorset Ball Clay m a s 850 806 - 66
946 + 19
Farnley Fireclay a s a 870 654 - 210
785 - 80
960 + 41
China Clay - a - >950 960 - 55
Q-quartz a = abundant > 30%
K-kaolinite s= subsidiary > 15% <30%
M-mica or illite m=minor > 5% < 15%
134 ARCHAEOMETRY
of the sintering characteristics of the sherd and measurements were also taken
whilst the specimen was cooling down to room temperature.
With the second specimen, the shrinkage temperature (Ta)was again determined
and the specimen was then refired, while still mounted in the dilatometer, at
temperature, T l , for 1 hour: the refiring temperature was chosen on the basis
of the sintering characteristics observed for the first specimen. After cooling to a
temperature approximately 300°C below the refiring temperature, the specimen
was reheated and the new shrinkage temperature, T:, was determined. The
“equivalent firing temperature” was estimated using equation (1).
In order to obtain some indication of the effect of absorbed moisture, a
selection of the specimens were, after refiring and measurement of shrinkage
temperature, T l , subjected to steam treatment at atmospheric pressure for
100 hours. After drying at 130°C, the thermal expansion measurements were
repeated and a further shrinkage temperature, T,”, was determined.
shrinkage due to the pressure exerted by the dilatometer components, rather than
to the resumption cf sintering, can occur. This effect was observed with a specimen
of electrical porcelain (T, = 1230°C) for which T, was increased by as much
as 100°C by reducing the pressure of the dilatometer rods on the specimen.
Consequently it is probable that the values obtained for T, were too low in the
case of some sherds fired at high temperatures (e.g. A25, 26, 27 and 28).
In principle therefore the “equivalent firing temperature” of Group A sherds
can be estimated using the refiring data in conjunction with equation (1). Errors
of 2 5 ° C in the measurement of TI, and T:, together with the approximate
nature of the correction for the effect of absorbed moisture, suggest that for a
single specimen the error in T,, is *2O0C, when the criterion that (Te’-T,J
equals 20-30°C is adequately satisfied. However when this criterion is not satisfied
(sherds A l , 3, 4, 6, 1.1, 18, 22, 25, 26, 27 and 28) or when the values of T, for
specimens cut from a single sherd differ by more than lO”C, the error in T,,
is greater. Furthermore no correctirn for bloating or the presence of an extensive
glass/liquid phase is possible.
4.2.2. Group B sherds. For the sherds in this group, it is unlikely that the
vitrification range of the clays was reached during the original firing since T, was
less than 650°C and in addition, with the exception of sherd B5, the expansion in
the 450-550°C range was reduced after heating to 850°C (i.e. CY,,/CY, > l ) . Conse-
quently determination of T,, using equation (1) is not valid and the thermal
expansion data must be interpreted in conjunction with information concerning
the mineralogical composition of the ceramics.
Sherd BZ. X-ray diffraction and d.t.a. measurements established that the
hydrated clay minerals, kaolinite and illite, were present and consequently
it is probable that the firing temperature was less than 500°C. However the
possibility that a higher firing temperature was employed and that rehydration
of the clay minerals occurred as a result of moisture absorption during burial
(Grim and Bradley 1948, Hill 1953), cannot be neglected. The value obtained
for T, provides no useful information since it was determined by the com-
pletion of expansion associated with dehydration of illitic clay minerals and
with the a - p quartz inversion.
Sheds B2, 3 and 4 (figure 2d). X-ray diffraction and d.t.a. measurements
established that no hydrated clay minerals were present and therefore it is
probable that the firing temperature was greater than 500°C. Since the value
obtained for T., provides no precise information, the results merely suggest
that the firing temperatures were in the 500-700°C range.
Sherd B5 (figure 2e). Shrinkage started below 100°C and was continuous
except for a very slight expansion at approximately 570°C due to the a - p
quartz inversion. The shrinkage was presumably associated with desorption of
moisture which had been absorbed during burial; similar results were observed
by Riley (1965), working with Egyptian ceramics. It is therefore only possible
to suggest a firing temperature in the 500-700°C range on the basis of the
absence of hydrated clay minerals and the fact that shrinkage became more
rapid above 650°C.
4.2.3. Group C sherds. Thermal expansion data does not provide a basis for
estimating T,, since with these sherds either the expansion prior to shrinkage was
extremely irregular or the shrinkage was followed by a large expansion (figure 2f).
X-ray diffraction and d.t.a. measurements established that calcite is present in
TABLE 111
Sherd Archaeological data Equivalent p i n g
no. Provenance Period 1Age Type temp. (T,* C)
Near East and Mediterranean Ceramics
A4 Mersin, Turkey Neolithic (c. - 750- 820
c1 Byblos, Lebanon Neolithic (c. So00 B1C.j - <800
A15 Arpachiyak, Iraq Chalcolithic (c. 4500 B.C.) Halaf ware 970- lO5Ot
c2 Chagar B a r , Syria Chalcolithic (c. 4500 B.C.) Halaf ware <800
A19 A1 'Ubaid, Iraq Bronze Age (c. 3500 B.C.', 'Ubaid ware ii40-ii80
A20 Ur, Iraq Bronze Age (c. 3500 B.C.j 'Ubaid ware 1070- 1110
B5 Erimi, Cyprus Chalcolithic (c. 3000 B.C.) - 500- 700
A14 Hala Sultan Tekke, Cyprus c. 1300 B.C. Mycenaean ware 940- 10007
A16 Myrtou, Cyprus c. 1300 B.C. Mycenaean copy 1030-10707
A17 A1 Mina, Turkey c. 500 B.C. Greek Attic ware 1OOo-1100
A18 A1 Mina, Turkey c. 500 B.C. Greek Attic ware 940- lOlOt
Roman Ceramics
c3 Dragonby, Lincs. Iron Age-Roman - <800
B3 Catterick, Yorks. Roman Spanish amphora 500- 700
B4 Castor, Hunts. Roman BIack burnished ware 500- 700
c4 Bainbridge, Yorks. Roman Calcite gritted ware <800
A6 Stibbington, Hunts. Roman Grey ware 900- 9607
A1 Hartshill, Wa+cks. Roman Mortarium : kiln 14a 600- 700
A8 Hafitshill, Wamcks. Roman Mortarium : kiln 5b 900- 950
A12 Hartshill, Warwicks. Roman Mortarium: kiln 15 930- 990
A13 Hafitshill, Warwicks. Roman Mortarium: kiln 2 950- 990
A7 Catterick, Yorks. Roman Colour coated ware 910- 980
A21 Catterick. Yorks. Roman Central Gaulish Samian 1020- 1090
A22 Catterick, Yorks. Roman Central Gaulish Samian 1 100- 1150
A23 Catterick, Yorks. Roman South Gaulish Samian 1100- 1150
A24 Lezoux, France Roman Central Oaulish Samian 1030-11307
Post-Roman Ceramics
B2 Baston, Lincs. Saxon - 500- 700
A10 Ipswich, Suffolk Saxon Thetford ware 920- 9607
A3 Olney, Bucks. Mediaeval - 620- 740
A2 Laverstock, Wilts. Mediaeval Kiln 2 750- 820
A1 1 West Cowick, Yorks. Mediaeval Kiln 1, level 4 940- 990t
A5 Pottersbury, Northants. c. 1650 A.D. Kiln 1B 910- 950
A9 Halifax, Yorks. c. 1650 A.D. Pule Hill kiln 910- 950
Miscellaneo~m
B1 Ilpox, Nigeria - Clay figurine <500
A25 China Sung dvnastv Porcelain i070-1140*
A26 China Sung (Chek:ang) dynasty Celadon 1070-1190'
A27 China - Porcelain : provincial 970 - 1060'
A28 China - .
Ching~.(K'ang- Hsi). dynasty Porcelain 960- 1050+
?Bloating: T,,possibly too high 'Extensive glassiliquid phase: T., possibly too low
ARCHAEOMETRY 141
the sherds. Since calcite decomposes in the 750-850°C range, it is probable that the
firing temperature was less than 800°C. However the possibility that a higher
firing temperature was employed and that hydration and subsequent recarbonation
of dissociated calcite occurred during burial, cannot be neglected. This uncertainty
could be resolved by optical examination of the sherds in thin section since, by
this technique, it is possible to distinguish the fine granular mass of the recarbonated
form from the unaltered calcite (Tobler 1939, Felts 1942).
4.3. Discussion
In Table 111, the values for the “equivalent firing temperatures” are presented
in the form of a temperature range which was determined on the basis of the
above considerations (Section 4.2). The archaeological data is included and
the sherds are grouped according to age and provenance.
From these results, i t can be seen that firing temperatures ranging from
500°C to 1200°C were used in the manufacture of ancient ceramics and that
low or high firing temperatures were not confined to particular periods or parts of
the world. In addition the following tentative comments can be made with respect
to specific groups of sherds : -
(i) The high firing temperatures (l05O-l20O0C)used in the manufacture of
Ubaid pottery (A19 and 20) confirms the results of Tobler (1939)who suggested
that some Ubaid pottery, found at Tepe Gawra in Iraq, had been fired to
1200°C since “grains of orthoclase in the sand filler had melted and had been
coated with a glass”.
(ii) Similar firing temperatures (950-1050°C) were employed in the manufacture
of pottery from Mycenae, itself (A14). and locally-produced copies found in
Cyprus (A16).
(iii) The firing temperatures employed during the Roman period ranged from
500-700°C for the coarse pottery, such as amphora (B3). to 1000-1200°Cfor
the high class Samian ware (A21,22,23and 24).
(iv) During the post-Roman period, a similar range of firing temperatures
to that for the Roman period was employed except that there were no ceramics,
in the group selected for this work, comparable in quality with the Samian ware.
(v) Although the results suggest that the firing temperatures for Chinese
porcelain (A25-28)were in the 950-1200°Crange, it is possible that because of
the presence of an extensive glass/liquid phase these values are too low.
Ancillary data for the interpretation of thermal expansion results was obtained
from the temperature measurements made during the firing of full-scale replicas
of Romano-British pottery kilns (Mayes 1961 and 1962). These kiln experiments
indicated that satisfactory ceramics could be produced if temperatures greater
than 850°C were maintained for approximately 1 hour and hence the values
for T,,, presented in Table 111. were calculated assuming an original firing time
of 1 hour.
In addition the kiln experiments showed that at the peak temperature (950°C),
the temperature at different points on the kiln floor varied by at least 100°C.
This observation, together with the fact that different values of T, were observed
for specimens cut from a single sherd. indicates that it would be dangerous
to aiiach too mu& arciiaeoiogical significance to a precise vaiue of T,, obtained
for a single sherd. This warning is especially important when the sherd is found
on the kiln site itself (eg. A l , 2, 5, 8, 9, 11, 12, 13 and 24) since in this case
142 ARCHAEOMETRY
the sherd has a greater probability of being a “waster”: that is a sherd which
has been over- or under-fired.
5. CONCLUSIONS
From the results presented in sections 3 and 4, it is apparent that the validity
and accuracy of the theimal expansion method for thc determination of the
firing temperature of ancient ceramics depends on the firing temperature employed
and the mineralogical composition of the clay.
When the shrinkage temperature is less than 700°C (i.e. no vitrification during
firing) or when the ceramic contains calcite, the thermal expansion data can only
provide a very approximate value for T,, and must be considered in conjunction
with the mineralogical data.
When the shrinkage temperature is greater than 700°C (i.e. vitrification during
firing) then a value for Teq, accurate to -t-20°C for a single specimen, can be
obtained from the thermal expansion data using equation (1); a firing time
of 1 hour being assumed. However even in this case, each result must be carefully
considered in order to establish the importance of further inaccuracies associated
with: -
(i) the possibility that the high value for T, is due to the fact that clays
with high illitic content do not contract until vitrification begins (Section 3.2).
(ii) failure to satisfy the criterion that (Te’- Trq)must equal 20-30°C (Section
3.1).
(iii) contraction, during thermal expansion measurements, due to desorption
of moisture absorbed during burial (Section 3.1.2).
(iv) bloating during thermal expansion measurements (Section 3.1.3).
(v) contraction, due to pressure exerted by the dilatometer components, when
the viscosity of the liquid phase decreases at high temperatures.
In conclusion therefore it can be stated that, with careful assessment of
the results, thermal expansion measurements provide a valuable method for
determining the firing temperature of ancient ceramics. Further measurements on
ceramics would add to the information on the performance of ancient kilns and
the technological capabilities of the potters, provided by the above results. In
addition measurements could be made on specimens taken from the kiln fabric
itself although assumptions concerning the firing time would be more hazardous
since each kiln has been used for a large, but unknown, number of firings.
ACKNOWLEDGEMENTS
In am extremely grateful to Professor J. P. Roberts for his active help and
encouragement in this work. I am indebted to Mr. R. Bluett. Dr. H. W. Catling,
Dr. E. T. Hall, Mr. and Mrs. B. R. Hartley, Mr. J . May, Mr. P. Mayes,
Dr. P. R. S . Moorey, Dr. J. Musty and Mr. F. Willett for providing the pottery
sherds and also to Woodside Brickworks Limited and Pike Bros., Fayle and
Company Limited for providing the clay samples.
Financial support for the project from the Science Research Council and an
I.C.I. Research Fellowship are gratefully acknowledged.
ARCHAEOMETRY 143
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