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Crystals
Special Issues
Archaeological Crystalline Materials
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Archaeological Crystalline Materials

A special issue of Crystals (ISSN 2073-4352). This special issue belongs to the section "Crystalline Materials".

Deadline for manuscript submissions: closed (16 December 2022) | Viewed by 13663

Special Issue Editors

Dr. Claudia Scatigno

E-Mail Website
Guest Editor
CREF—Museo Storico della Fisica e Centro Studi e Ricerche Enrico Fermi, Via Panisperna 89a, 00189 Rome, Italy
Interests: data analysis (machine learning, computing, modelling); physics applied: spectroscopy (optical and neutron); analytical and environmental chemistry (air quality, sensors, environmental monitoring); molecular science
Special Issues, Collections and Topics in MDPI journals
Dr. Giulia Festa

E-Mail Website
Guest Editor
CREF - Museo Storico della Fisica e Centro Studi e Ricerche “Enrico Fermi”, Via Panisperna 89 a, c/o Piazza del Viminale 1, 00189 Rome, Italy
Interests: neutron and X-rays techniques for cultural heritage; neutron and X-ray imaging; diffraction; gamma spectroscopy; neutron resonance analysis; Raman spectroscopy and X-ray fluorescence
Special Issues, Collections and Topics in MDPI journals
Prof. Dr. Maite Maguregui

E-Mail Website
Guest Editor
Department of Analytical Chemistry, Faculty of Pharmacy, University of the Basque Country UPV/EHU, Paseo de la Universidad 7, 01006 Vitoria-Gasteiz, Spain
Interests: heritage science; effects of environmental factors, climate change, and natural hazards on the conservation of cultural heritage; salt crystallization in building materials; hybrid materials for the conservation of cultural heritage; in-situ and laboratory non-invasive analytical methodologies; environmental science; planetary science

Special Issue Information

Dear Colleagues,

The crystalline state of archaeological materials from bioarchaeological and paleontological materials (bones, seeds, etc.) to building remains (decorative archaeological pigments, wall paintings, mosaics, furnishings), and other archaeological records (ceramics, sculptures, lithic materials, etc.) undergo changes in lattice parameter and crystalline domain size because of diagenetic alteration or exposure to the atmosphere. To diagnose and study these alterations, an increasing effort from the scientific community is required. Portable instruments and non-destructive analyses should always be preferable. Recently, the quality of the data output of these new portable systems has become competitive with the conventional benchtop methods. Moreover, data science and machine learning (e.g., the predictive modelling of multivariate analysis, multivariate regression algorithms) have recently been adopted to address open questions dealing with provenance, technological features, and state of conservation.

The present Special Issue on “Archaeological Crystalline Materials” offers researchers in the field of heritage science the opportunity to present new analytical approaches and tools able to identify and quantify (if possible) the transformation of crystalline phases in archaeological records. At the same time, the aim of this Issue is to be able not only to monitor the transformation, but also to identify the role of natural/anthropogenic contaminants in the burial and the influence of environmental forces in the conservation of archaeological materials.

Dr. Claudia Scatigno
Dr. Giulia Festa
Prof. Dr. Maite Maguregui
Guest Editors

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Crystals is an international peer-reviewed open access monthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2600 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • archaeological records
  • crystalline phases transformation
  • phase identification and quantification
  • in situ and laboratory analysis
  • data science and machine learning
  • diagnosis of the state of conservation
  • diagenetic alterations in the burial
  • interaction with the atmosphere
  • natural and anthropogenic environmental agents

Published Papers (8 papers)

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Research

13 pages, 7184 KiB  
Article
Contribution to the Understanding of Mural Painting Techniques of Jinpari Tomb No. 4 of the Complex of Koguryo Tombs, World Heritage
by Hwa Soo Lee and Kyeong Soon Han
Crystals 2023, 13(3), 459; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst13030459 - 07 Mar 2023
Cited by 1 | Viewed by 1207
Abstract
In this study, we have analyzed the chemical components and crystal structures of minerals found in the Jinpari Tomb No. 4 mural paintings, which has allowed us to identify component materials comprising each layer. During the analysis of the painting layer, the green [...] Read more.
In this study, we have analyzed the chemical components and crystal structures of minerals found in the Jinpari Tomb No. 4 mural paintings, which has allowed us to identify component materials comprising each layer. During the analysis of the painting layer, the green material was identified as malachite. The use of malachite is supported by the high Cu content, the flower-shaped crystals in the microstructures of the painting layer, and the XRD identification results. The ground layer consists of layers of panel-shaped particles. The main component materials were Ca, Al, Si, K, Mg, and Fe, which are usually found in earthen materials. The earthen layer showed high peaks of silicon oxide and calcium carbonate, along with potassium aluminum silicate. The findings indicate quartz, limestone, and mica. The lime layer showed the diffraction patterns corresponding to calcium carbonate, which indicates the use of limestone. The earthen layer consists of aggregated layers of thin panel-shaped structures, with small particles attached around the structures. The lime layer showed aggregations of multi-angle panel-shaped structures and pillar-shaped structures of various types. The analysis has allowed us to shed light on the techniques used in the Jinpari Tomb No. 4 mural paintings. Full article
(This article belongs to the Special Issue Archaeological Crystalline Materials)
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17 pages, 5138 KiB  
Article
New Insights into the Geochemical Processes Occurring on the Surface of Stuccoes Made of Slaked Lime Putty
by Luciana Pocostales, Àfrica Pitarch Martí, Núria Guasch-Ferré, María Teresa Doménech-Carbó and José Luís Prada Pérez
Crystals 2023, 13(2), 219; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst13020219 - 24 Jan 2023
Viewed by 1068
Abstract
The fresco technique performed with slaked lime putty as binding material has been well known since Antiquity. However, the geochemical processes that occur on the surface have been generally described as part of the carbonation process of the intonaco itself. When approaching this [...] Read more.
The fresco technique performed with slaked lime putty as binding material has been well known since Antiquity. However, the geochemical processes that occur on the surface have been generally described as part of the carbonation process of the intonaco itself. When approaching this technique from experimental archaeology, it has been observed for the first time that during the execution period (from 0 to 20 h, approximately) the processes occurring on the surface of the stucco are different from those occurring inside. Furthermore, these processes lead to the formation of an epigenetic film of specific texture, stiffness and compactness. This study investigates the formation and evolution of this surface film using a series of slaked lime putty stucco test tubes. Samples were extracted at different intervals and subsequently analyzed by polarized optical microscopy, scanning electron microscopy, and Fourier transform infrared spectroscopy. Results indicate that the development of the film, composed of an amorphous gel-like stratum and a micro-crystalline stratum, occurs in parallel to the carbonation occurring inside the stucco. Moreover, this process does not respond to the classical geological processes of calcium carbonate formation. It was also observed that its presence slows down the carbonation in the underlying strata (intonaco, intonachino, arriccio, etc.) and that the surface becomes more crystalline over time. The identification of this film has implications for the field of the conservation–restoration of fresco paintings and lime-based wall paintings. Full article
(This article belongs to the Special Issue Archaeological Crystalline Materials)
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16 pages, 8914 KiB  
Article
A Non-Invasive In Situ Spectroscopic Analysis of Cinnabar Minerals to Assist Provenance Studies of Archaeological Pigments
by Silvia Pérez-Diez, Cheyenne Bernier, Javier G. Iñañez and Maite Maguregui
Crystals 2023, 13(2), 207; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst13020207 - 23 Jan 2023
Viewed by 1585
Abstract
This study presents a non-invasive in situ methodology based on the use of portable elemental (energy dispersive X-ray fluorescence spectroscopy, EDXRF) and molecular (Raman spectroscopy) spectroscopic-based instrumentation as a tool to obtain preliminary information to assist subsequent provenance studies of archaeological cinnabar pigments [...] Read more.
This study presents a non-invasive in situ methodology based on the use of portable elemental (energy dispersive X-ray fluorescence spectroscopy, EDXRF) and molecular (Raman spectroscopy) spectroscopic-based instrumentation as a tool to obtain preliminary information to assist subsequent provenance studies of archaeological cinnabar pigments in the laboratory. In this work, six cinnabar mineral ores, extracted from the Almadén mining district and an original raw pigment coming from the Archaeological Park of Pompeii have been analyzed. As the detection capacities and spectral resolution of the portable instruments are usually poorer than the equivalent benchtop equipment, a comparative study of the in-situ and laboratory results was conducted. Afterward, chemometric data treatment was performed considering both the molecular and elemental information. According to the elemental results, it was not possible to find a strong concordance between the cinnabar ores and the pigment from Pompeii, suggesting the need for additional methodologies in the laboratory (isotope ratio analysis) to complete a proper provenance study. However, this approach was useful to classify the ores according to their mineralogical differences. Therefore, this methodology could be proposed as a useful tool to conduct a representative sampling of the cinnabar mineral ores to be considered in a provenance study of archaeological cinnabar pigments. Full article
(This article belongs to the Special Issue Archaeological Crystalline Materials)
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18 pages, 1497 KiB  
Article
SiO2 Nanoparticles as New Repairing Treatments toward the Pietraforte Sandstone in Florence Renaissance Buildings
by Federica Valentini, Pasquino Pallecchi, Michela Relucenti, Orlando Donfrancesco, Gianluca Sottili, Ida Pettiti, Valentina Mussi, Sara De Angelis, Claudia Scatigno and Giulia Festa
Crystals 2022, 12(9), 1182; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst12091182 - 23 Aug 2022
Cited by 2 | Viewed by 1524
Abstract
In this work, the consolidation efficiency of SiO2 nanoparticles (synthesized in the Chemistry laboratories at the Tor Vergata University of Roma) was tested on Pietraforte sandstone surfaces belonging to the bell tower of San Lorenzo (Florence, Italy) and was fully investigated. Nanoparticles [...] Read more.
In this work, the consolidation efficiency of SiO2 nanoparticles (synthesized in the Chemistry laboratories at the Tor Vergata University of Roma) was tested on Pietraforte sandstone surfaces belonging to the bell tower of San Lorenzo (Florence, Italy) and was fully investigated. Nanoparticles (synthesized in large-scale mass production) have been characterized by XRD—X-Ray Diffraction; Raman and FTIR—Fourier Transform Infrared spectroscopy; SEM—Scanning Electron Microscopy; while the Pietraforte sandstone morphology was examined by Porosimetry, capillary absorption test, surface hardness test, drilling resistance and tensile strength. The colorimetric measurements were also performed to characterize the optical modification exhibited by Pietraforte sandstones, especially after the SiO2 treatments. Our results show that applying to the Pietraforte, the new consolidating agent based on SiO2 nanoparticles, has several advantages, as they are more resistant to perforation, wear, and abrasion even long range (for long times of exposure and consolidating exercise against Florentine sandstone), compared to the CaCO3 nanoparticles (tested in our previous paper), which instead show excellent performance but only close to their first application. This means that over time, their resistance to drilling decreases, they wear much more easily (compared to SiO2-treated sandstone), and tend to exhibit quite a significant surface abrasion phenomena. The experimental results highlight that the SiO2 consolidation efficiency on this kind of Florentine Pietraforte sandstone (having low porosity and a specific calcitic texture) seems to be higher in terms of water penetration protection, superficial cohesion forces, and an increase in surface resistance. Comparing the performance of SiO2 nanoparticles with commercial consolidants in solvents such as Estel 1000 (tested here), we demonstrate that: (A) the restorative effects are obtained with a consolidation time over one week, significantly shorter when compared to the times of Estel 1000, exceeding 21 days; (B) SiO2 nanoparticles perform better than Estel 1000 in terms of cohesion forces, also ensuring excellent preservation of the optical and color properties of the parent rock (without altering it after application). Full article
(This article belongs to the Special Issue Archaeological Crystalline Materials)
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13 pages, 3992 KiB  
Article
Barium Hydroxide Nanoparticle–Phosphoric Acid System for Desalination and Consolidation of Tomb Murals
by Yan Rong, Jinglong Yang, Siping Huang and Yuhu Li
Crystals 2022, 12(8), 1171; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst12081171 - 20 Aug 2022
Cited by 1 | Viewed by 1721
Abstract
Tomb murals are an important component of cultural heritage, but the extant majority of burial murals are severely damaged. There are various causes behind the deterioration of tomb murals, among which the detrimental effects of sodium sulfate on murals are some of the [...] Read more.
Tomb murals are an important component of cultural heritage, but the extant majority of burial murals are severely damaged. There are various causes behind the deterioration of tomb murals, among which the detrimental effects of sodium sulfate on murals are some of the most difficult to treat. In the past decades, the application of alkaline earth metal hydroxides (such as Ba(OH)2, Ca(OH)2, and Ma(OH)2) for the conservation and consolidation of murals has become more common. However, there are some problems, such as large particles, poor permeability, and potential for surface whitening. In response to this issue, we investigated a facile method for the synthesis of nano barium hydroxide (N-Ba(OH)2), from which we developed a barium hydroxide nanoparticle–phosphoric acid (N-Ba(OH)2/H3PO4) multisite in situ consolidation system. The results show that N-Ba(OH)2/H3PO4 consolidation material has good permeability and mechanical properties compared with commercial Ba(OH)2 and other common consolidation materials. This material performs very well in both salt resistance and desalination tests, the color difference change is minimal, and the technique is suitable for the practical manipulation of outdoor artifact conservation work. Recently, it has even been used in the desalination and consolidation of tomb murals in Jiangxi, China, the results of which opened a new way of thinking about the long-term conservation of tomb murals. Full article
(This article belongs to the Special Issue Archaeological Crystalline Materials)
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13 pages, 8075 KiB  
Article
Wall Materials and Manufacturing Techniques for Korean Ancient Mural Paintings (Great Gaya, 6th Century)—Discovery of Shells Used in Wall Plaster and Identification of Their Processing Status
by Hwa Soo Lee, Yeong Gyeong Yu, Han Hyoung Lee and Kyeong Soon Han
Crystals 2022, 12(8), 1051; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst12081051 - 28 Jul 2022
Cited by 4 | Viewed by 1481
Abstract
This study used morphological analysis to identify the materials used for the wall plaster in the Goa-ri Tomb and elucidate the wall manufacturing techniques by determining the processing conditions for the plaster ingredients through a calcination experiment. A glossy nacreous layer (or folia [...] Read more.
This study used morphological analysis to identify the materials used for the wall plaster in the Goa-ri Tomb and elucidate the wall manufacturing techniques by determining the processing conditions for the plaster ingredients through a calcination experiment. A glossy nacreous layer (or folia layer) and an adductor muscle scar were identified on the ventral of the shell. The shell section was confirmed in the form of a lens-like prismatic layer (or chalky layer) inserted between the nacreous layer (or folia layer). The calcinated samples showed clusters of polygonal particles of different sizes. The experiment confirmed a process of particles in plate-type–bedded structures converting into shapeless particles followed by recrystallization. The samples calcinated at 650 °C and 750 °C mostly showed plate-type–bedded structures. According to the results of the study, the plaster used on the Goa-ri Tomb walls was confirmed to be made of oyster shells. The existence of many incompletely calcinated shell particles in the plaster indicates that the calcination temperature was not high enough or the heat was not evenly distributed. The Goa-ri Tomb used weaker and less durable plaster made of incompletely calcinated shells, which seems to have caused the extensive exfoliation of the plaster from the wall surfaces. Full article
(This article belongs to the Special Issue Archaeological Crystalline Materials)
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17 pages, 14361 KiB  
Article
Macroscopic and Petrographic Analyses of the Mortars from the Roman villa of Noheda (Villar de Domingo García, Cuenca)
by Miguel Ángel Valero Tévar, Xoan Moreno Paredes, Pablo Guerra García, Xabier Arroyo Rey and Nelia Valverde Gascueña
Crystals 2022, 12(5), 606; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst12050606 - 25 Apr 2022
Cited by 1 | Viewed by 1498
Abstract
The Roman villa of Noheda, located in the municipality of Villar de Domingo García (Cuenca), is one of the most important archaeological sites in Spain and one of the most important museum complexes in Europe. In recent years, several archaeological investigations have been [...] Read more.
The Roman villa of Noheda, located in the municipality of Villar de Domingo García (Cuenca), is one of the most important archaeological sites in Spain and one of the most important museum complexes in Europe. In recent years, several archaeological investigations have been developed (archaeometry of building materials, natural resources, ways and roads). Furthermore, various restoration and consolidation works have been carried out on structures, walls and floors. The archaeological management team requested a characterisation of the mortars found in the coatings of the walls and floors of the complex to identify differences in its production. After checking the rooms, the state of conservation of the elements and the significance of the materials used, several mortar samples were analysed by means of macroscopic techniques before applying a petrographic analysis. The results showed an interesting variety in the distribution of aggregates, a complex microstratigraphy and a range of grain sizes in the mortars from different rooms. Magnesium, silica and aluminium from limestone were found. Crushed and powdered limestone was used as an aggregate with irregular distribution. Calcite nodules were observed as evidence that the mortar had been poorly mixed in preparation. Full article
(This article belongs to the Special Issue Archaeological Crystalline Materials)
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26 pages, 5751 KiB  
Article
Non-Invasive Approach to Investigate the Mineralogy and Production Technology of the Mosaic Tesserae from the Roman Domus of Villa San Pancrazio (Taormina, Italy)
by Olivia Gomez-Laserna, Anna Irto, Pablo Irizar, Gabriele Lando, Clemente Bretti, Irantzu Martinez-Arkarazo, Lorenzo Campagna and Paola Cardiano
Crystals 2021, 11(11), 1423; https://0-doi-org.brum.beds.ac.uk/10.3390/cryst11111423 - 21 Nov 2021
Cited by 1 | Viewed by 1989
Abstract
The archaeological excavations at Villa San Pancrazio (Taormina, Italy) are bringing to light a vast Roman-Imperial residential quarter featuring luxurious dwellings decorated with wall paintings and mosaic floors, pointing it out as one of the most significant archaeological sites of the city. The [...] Read more.
The archaeological excavations at Villa San Pancrazio (Taormina, Italy) are bringing to light a vast Roman-Imperial residential quarter featuring luxurious dwellings decorated with wall paintings and mosaic floors, pointing it out as one of the most significant archaeological sites of the city. The polychrome and black and white mosaics recovered date back to the middle Imperial period, during the 2nd century AD. This work deals with the first archaeometric investigations of the materials employed for the tesserae production with the aim of elucidating the mineralogical composition and obtaining analytical evidence that can contribute to extracting information related to their production technology. For that purpose, a non-invasive methodology, based on micro energy dispersive X-ray fluorescence (μ-EDXRF) spectrometry and Raman spectroscopy, was used to characterize a wide selection of stone, ceramic and glass tesserae. Chemometric tools were exploited to manage the large set of elemental data collected on black and white lithic samples, providing essential clues for the subsequent investigations. The results evidenced the employment of natural lithotypes (calcareous sedimentary, dolomitic and volcanic) local and imported, and also artificial materials, such as ceramic made firing magnesium-rich clays, soda-lime-silica glasses made with different opacifying and coloring agents (such as calcium antimoniate, cobalt and copper). Full article
(This article belongs to the Special Issue Archaeological Crystalline Materials)
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