Aleksandr S. Pakhunov^1,2,3,*, Roman D. Svetogorov^4,**, Alexey V. Ovcharov^4,***, Mikhail N. Shushunov^4,****, Roman A. Senin^4,*****

¹Institute of Archaeology RAS, Moscow, Russia
²Novosibirsk State University, Russia
³University of Bordeaux, France
⁴“Kurchatov Institute” National Research Centre, Moscow, Russia
*E-mail: science@pakhunov.com
**E-mail: Svetogorov_RD@nrcki.ru
***E-mail: ovcharov.91@gmail.com
****E-mail: viggenin@yandex.ru
*****E-mail: senin_ra@nrcki.ru

Keywords: the Upper Paleolithic, the Kapova cave, pigments, heat treatment, scanning electron microscopy, transmission electron microscopy, synchrotron powder X-ray diffraction.

Pigments are widely occurring in the Kapova cave. They can be found in the cultural layers in different chambers and on the floor of the cave, while “crayons” were found only in the cultural layer in the Chamber of Signs. Ten largest fragments of ochre and one sample of powdered pigment from the cultural layer, excavated by V.E. Shchelinsky in 1986, were analyzed. The presence of a large number of ochre pieces, powder and largely coloured cultural layer indicate that technological operations to prepare the pigment were conducted in the studied areas. The samples are fragments of red colour pigment in different shades. The shape of the six of them suggests that they were used to prepare the powdered pigment by grinding. The analysis of mineral composition showed the presence of goethite and hematite in most of the red samples in different ratios. Particles of goethite and hematite were also simultaneously detected in one of the samples with the use of transmission electron microscopy, which made it possible to determine the stage of goethite dehydration. The microscopic study showed that most hematite particles have a disordered structure with the presence of slit-like pores of nanometer size. In addition, this study revealed the beginning of the rounded pore formation which is characteristic of the initial phase of goethite to hematite transformation. These features are evidence of short-term low-temperature (up to 400°C) annealing near the campfire, which caused partial dehydration of goethite. That fact confirms previous suggestions that firing was used to obtain red pigment. The obtained data will be applied for a comparative analysis of pigments from the paintings in order to determine the technological process of pigments production and to find evidence of heat treatment in pigments from other chambers of the cave.

DOI: 10.31857/S086960630013700-9