Methodological aspects of SANS and TOF neutron diffraction measurements on pottery: the case of Miseno and Cuma A. Botti a, * , M.A. Ricci a , G. De Rossi b , W. Kockelmann c , A. Sodo d a Dipartimento di Fisica E. Amaldi, Universita ` degli Studi Roma Tre, and INFM, Unita ` Roma Tre, Via della Vasca Navale 84, 00146 Roma, Italy b Via Casilina Km 22.800, Monte Compatri, Italy c ISIS Facility, Rutherford Appleton Laboratory, Chilton, Didcot OX11 0QX, UK d ESRF, Grenoble Cedex 38000, France Received 26 November 2004; received in revised form 5 May 2005; accepted 22 June 2005 Abstract Small angle neutron scattering and neutron phase analysis techniques have been for the first time jointly employed to extract microscopic parameters of ceramic samples prepared under controlled conditions, in an attempt to establish a protocol for deriving information on the firing process. Data have also been collected on two series of early medieval samples from the Italian regions of Cuma and Miseno. The variation of the microscopic features observed on these samples could mirror some technological evolution in the period spanning from the 6th to the 12th century AD. Ó 2005 Elsevier Ltd. All rights reserved. Keywords: Small angle neutron scattering; Phase analysis; Medieval pottery 1. Introduction Neutron scattering is a promising method for the anal- ysis of bulk materials due to its versatility and non- destructivity [33]. Neutrons can indeed penetrate deeply inside matter, since they are not charged and interact with the nuclei via short range forces. As a consequence, bulky samples and in particular pottery artefacts can be inves- tigated in principle without any specific preparation. The information delivered by the neutrons scattered by a sample concerns both the spatial organization of the atomic units and their dynamics. Here we will focus on techniques which probe the structure of the sample at a microscopic and mesoscopic level, to investigate intact ceramic artefacts and pottery sherds. The description of the bulk properties of ceramic samples, such as pottery finds, can indeed be done in terms of a hierarchy of struc- tures of growing size, going from the elements [12,13,34], to the mineral phases [20,36,37], the aggregates, the texture pattern [17], the petrographic properties [24,28] and finally the macroscopic inhomogeneities [3,7,8,29]. X-Ray Diffraction (XRD) [26,31,39] and Neutron Diffraction (ND) [20] contribute an important progress in recognizing and classifying the sherds. Both give access to the distribution of mineral phases and their relative weights in the phase mixture, to the crystal structures of the individual phases and to the orientational distribu- tion of grains. X-rays are suitable for studying powders and surfaces, whereas neutrons can be used on the intact object for quantitative analysis. In order to move one step forward in the length scale hierarchy, and investigate the characteristics of mineral aggregates Small Angle X-ray Scattering (SAXS) and Small Angle Neutron Scattering (SANS) are needed. SAXS technique has been applied * Corresponding author. E-mail address: botti@fis.uniroma3.it (A. Botti). 0305-4403/$ - see front matter Ó 2005 Elsevier Ltd. All rights reserved. doi:10.1016/j.jas.2005.06.016 Journal of Archaeological Science 33 (2006) 307e319 http://www.elsevier.com/locate/jas