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A special issue of Materials (ISSN 1996-1944). This special issue belongs to the section "Advanced Materials Characterization".

Deadline for manuscript submissions: closed (20 December 2022) | Viewed by 24627

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Prof. Dr. Žiga Šmit

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1. Faculty of Mathematics and Physics, University of Ljubljana, SI-1000 Ljubljana, Slovenia
2. Jožef Stefan Institute, SI-1000 Ljubljana, Slovenia
Interests: ion beam analysis; archaeological glass and metals; ionization models
Special Issues, Collections and Topics in MDPI journals

Dr. Eva Menart

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Guest Editor

1. National Museum of Slovenia, SI-1000 Ljubljana, Slovenia
2. Jozef Stefan Institute, SI-1000 Ljubljana, Slovenia
Interests: non-destructive analysis; cultural heritage objects; material degradation; preventive conservation
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

A Special Issue of Materials is devoted to the studies in the field of cultural heritage. Our ancestors have left us numerous spiritual and material remains and artefacts, and their understanding is important for functioning of the modern society. We are then bound to preserve and study our cultural heritage, which is quite challenging even by modern analytical methods. We therefore welcome all contributions that are dealing with studies of cultural heritage preservation and with analytical studies that would help us understand how our ancestors obtained raw materals, what production techniques they applied, how they traded with their products, how they used them and why some of them virtually accompanied them in their afterlife. Material analysis of heritage objects would then help us understand economic, political and social relations in ancient societies.

The authors are invited to sumbit manuscripts on the following themes:

Environmental monitoring of the CH storage and display areas
Degradation studies on the objects of CH
Innovative conservation procedures
Authenticity testing of CH objects and detection of forgery
Application of dating techniques
Development of specialized analytical techniques
Studies of specific materials: arhaeological glass, metals, pigments, lithic materials
Experimental archaeology, i.e., reconstruction of ancient techniques and materials

Prof. Dr. Žiga Šmit
Dr. Eva Menart
Guest Editors

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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. Materials is an international peer-reviewed open access semimonthly journal published by MDPI.

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Keywords

analytical techniques in cultural heritage studies

Published Papers (12 papers)

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Editorial

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2 pages, 198 KiB

Open AccessEditorial

Special Issue of “Material Analysis in Cultural Heritage”

by Žiga Šmit and Eva Menart

Materials 2023, 16(6), 2370; https://0-doi-org.brum.beds.ac.uk/10.3390/ma16062370 - 16 Mar 2023

Viewed by 899

Abstract

The objects of cultural heritage represent memories of human activities from the past [...] Full article

(This article belongs to the Special Issue Material Analysis in Cultural Heritage)

Research

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19 pages, 4720 KiB

Open AccessArticle

Characterization of In Situ Concrete of Existing RC Constructions

by Marco Vona

Materials 2022, 15(16), 5549; https://0-doi-org.brum.beds.ac.uk/10.3390/ma15165549 - 12 Aug 2022

Cited by 3 | Viewed by 1098

Abstract

The strengths and mechanical characteristics of concrete play a key role in the safety levels for the recovery and reuse of existing RC buildings and civil engineering works. This is one of the main focuses of the current research trend. To this aim, the characteristics of concrete must be investigated: the characterization of the concrete and its in situ conditions play a key role. For these reasons, many studies on in situ and laboratory test methods and procedures have been carried out over the last two decades. In the past few years, non-destructive investigation methods have been considered reliable and used in many engineering applications, also for RC constructions. More recent codes and guidelines identify destructive test methods as a reference for practice application. However, non-destructive investigation methods can be used though exclusively in combination with destructive tests to support them. In this study, a significant database is considered to assess the reliability of the relationship between destructive and non-destructive methods for in situ concrete in existing RC constructions. The results of the analyses are used to verify the effectiveness of the methods and prediction models and suggest more effective test procedures. It can be stated that many of the existing empirical methods (based on pre-established correlations) are unable to provide a reliable evaluation of the compressive concrete strength and its variability. In practical applications, non-destructive methods often lead to unsatisfactory results for the existing reinforced concrete constructions. Finally, based on the results, some first operational indications are provided for practical investigations and future possible codes and guideline improvements. Full article

(This article belongs to the Special Issue Material Analysis in Cultural Heritage)

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17 pages, 15270 KiB

Open AccessArticle

Degradation of CdS Yellow and Orange Pigments: A Preventive Characterization of the Process through Pump–Probe, Reflectance, X-ray Diffraction, and Raman Spectroscopy

by Francesca Assunta Pisu, Pier Carlo Ricci, Stefania Porcu, Carlo Maria Carbonaro and Daniele Chiriu

Materials 2022, 15(16), 5533; https://0-doi-org.brum.beds.ac.uk/10.3390/ma15165533 - 11 Aug 2022

Cited by 2 | Viewed by 1622

Abstract

Cadmium yellow degradation afflicts numerous paintings realized between the XIXth and XXth centuries. The degradation process and its kinetics is not completely understood. It consists of chalking, lightening, flaking, spalling, and, in its most deteriorated cases, the formation of a crust over the original yellow paint. In order to improve the comprehension of the process, mock-up samples of CdS in yellow and orange tonalities were studied by means of structural analysis and optical characterization, with the principal techniques used in the field of cultural heritage. Mock ups were artificially degraded with heat treatment and UV exposure. Relevant colorimetric variation appears in CIE Lab coordinates from reflectance spectra. XRD, SEM-EDS, and Raman spectroscopy revealed the formation of cadmium sulfate, whilst time-resolved photoluminescence and pump–probe transient absorption spectroscopy suggest the formation of a defective phase, compatible with Cd vacancies and the formation of both CdO and CdSO₄ superficial clusters. Full article

(This article belongs to the Special Issue Material Analysis in Cultural Heritage)

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12 pages, 4623 KiB

Open AccessArticle

Position-Sensitive Bulk and Surface Element Analysis of Decorated Porcelain Artifacts

by László Szentmiklósi, Boglárka Maróti, Szabolcs Csákvári and Thomas Calligaro

Materials 2022, 15(15), 5106; https://0-doi-org.brum.beds.ac.uk/10.3390/ma15155106 - 22 Jul 2022

Cited by 4 | Viewed by 1304

Abstract

Non-destructive characterization of decorated porcelain artifacts requires the joint use of surface-analytical methods for the decorative surface pattern and methods of high penetration depth for bulk-representative chemical composition. In this research, we used position-sensitive X-ray Fluorescence Spectrometry (XRF) and Prompt-gamma activation analysis (PGAA) for these purposes, assisted by 3D structured-light optical scanning and dual-energy X-ray radiography. The proper combination of the near-surface and bulk element composition data can shed light on raw material use and manufacturing technology of ceramics. Full article

(This article belongs to the Special Issue Material Analysis in Cultural Heritage)

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15 pages, 18462 KiB

Open AccessArticle

Corrosion Layers on Archaeological Cast Iron from Nanhai I

by Minghao Jia, Pei Hu and Gang Hu

Materials 2022, 15(14), 4980; https://0-doi-org.brum.beds.ac.uk/10.3390/ma15144980 - 18 Jul 2022

Cited by 3 | Viewed by 1774

Abstract

Archaeological iron objects were excavated from the Nanhai I ship from the Southern Song Dynasty that sunk in the South China Sea. Most of these artifacts were severely corroded and fragmented. In order to understand their current corrosion state and guide their restoration and protection, optical microscopy, scanning electron microscopy, micro-laser Raman spectroscopy, infrared spectroscopy and X-ray diffraction were all selected for analysis. It was clear that the archaeological iron material was hypereutectic white iron with a carbon content of about 4.3–6.69%, and had experienced low-melt undercooling. There were many internal cracks formed by general corrosion that extended to the iron core, which tended to make the material unstable. At the interface between the iron and rust, there was a black dense layer enriched with chlorine, and a loose yellow outer layer. The dense layer was mainly composed of magnetite, akaganeite and maghemite, while the rust of the loose layer was composed of lepidocrocite, goethite, feroxyhite, maghemite and hematite. The major phases of all corrosion products were akaganeite and lepidocrocite. Numerous holes and cracks in the rust layer exhibited no barrier ability to the outside electrolyte, hence the iron core formed many redox electrochemical sites for general corrosion with the rust. Meanwhile, the dense rust located close to the iron core was broken locally by an enriched chlorine layer that was extremely detrimental to the stability of the archaeological iron. Using electrochemical impedance spectroscopy, it could be determined that the rust layers had no protective effect on the internal iron core under conditions of simulated seawater, and these rust layers even accelerated the corrosion. A mechanism for the rust growth as a result of laboratory testing was proposed to explain the entire corrosion process. In view of the desalination preservation treatment that had been applied for ten years, it was not recommended to maintain a single desalination operation. The archaeological rusted iron of the Nanhai I ship that was excavated from the marine environment should be properly stabilized and protected using corrosion inhibition and rust transformation for iron oxyhydroxides, since the rust structure and the internal iron core retain well together. Full article

(This article belongs to the Special Issue Material Analysis in Cultural Heritage)

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9 pages, 23521 KiB

Open AccessArticle

The Cultural Heritage of “Black Stones” (Lapis Aequipondus/Martyrum) of Leopardi’s Child Home (Recanati, Italy)

by Patrizia Santi, Stefano Pagnotta, Vincenzo Palleschi, Maria Perla Colombini and Alberto Renzulli

Materials 2022, 15(11), 3828; https://0-doi-org.brum.beds.ac.uk/10.3390/ma15113828 - 27 May 2022

Cited by 2 | Viewed by 1325

Abstract

A macroscopic lithological study and physical (hardness, size, weight) investigations, coupled with laser-induced breakdown spectroscopy (LIBS) and X-ray fluorescence (XRF) chemical analyses of three egg- and one pear-shaped polished black stones, exposed in the library of the child home of the famous poet Giacomo Leopardi, at Recanati (Italy), were carried out. They are characterized by different sizes: two with the same weight of 16.9 kg and the two smaller ones of 5.6 kg each, corresponding to multiples of standard roman weights (drachma and scrupulum). These features and the presence of some grooves on the rock artefacts, probably for grappling hooks, suggest an original use as counterweight for the four black stones herein classified as amphibole-bearing serpentinites whose lithologies are far away from Recanati (probably coming from geological outcrops in Tuscany). The four serpentinite stones closely match with the so-called Lapis Aequipondus used in antiquity by the Romans as counterweights. Due to the presence of lead rings or iron hooks in these stones, Lapis Aequipondus were also used for martyrdoms during the persecution of Christians in the Roman period, attached to the necks of martyrs that were then thrown in the wells or attached to the ankles of hanging bodies. This is the reason why these stones are also known as Lapis Martyrum, venerated with the relative martyrs, in several churches of Rome. The four black stones investigated probably arrived at Recanati from Rome after the middle of the 19th century. In the past, Christians also called Lapis Martyrum the “devil’s stones” (Lapis Diaboli). This could also be the reason for the popular belief that black stones cannot be touched by people, except those of the Leopardi dynasty. This work contributes to the cultural heritage of Leopardi’s child home, as the four black stones had never been investigated. Full article

(This article belongs to the Special Issue Material Analysis in Cultural Heritage)

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15 pages, 1335 KiB

Open AccessArticle

Shedding Light on Roman Glass Consumption on the Western Coast of the Black Sea

by Roxana Bugoi, Alexandra Ţârlea, Veronika Szilágyi, Ildikó Harsányi, Laurenţiu Cliante, Irina Achim and Zsolt Kasztovszky

Materials 2022, 15(2), 403; https://0-doi-org.brum.beds.ac.uk/10.3390/ma15020403 - 06 Jan 2022

Cited by 4 | Viewed by 1749

Abstract

The chemical composition of 48 glass finds from Histria and Tomis, Romania, chiefly dated to the 1st–4th c. AD, was determined using prompt gamma activation analysis (PGAA) at the Budapest Neutron Centre (BNC). Most fragments have composition typical for the Roman naturally colored blue-green-yellow (RNCBGY) glass; Mn-colorless, Sb-colorless, and Sb–Mn colorless glass finds were evidenced, too. Several Foy Série 2.1 and Foy Série 3.2 glass fragments, as well as an HIMT and a plant ash glass sample, were identified in the studied assemblage. The archaeological evidence, the glass working waste items, and the samples with compositional patterns suggestive of recycling are proofs of the secondary glass working activities at Tomis during the Early Roman Empire period. Full article

(This article belongs to the Special Issue Material Analysis in Cultural Heritage)

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26 pages, 8509 KiB

Open AccessArticle

The Technology Transfer from Europe to China in the 17th–18th Centuries: Non-Invasive On-Site XRF and Raman Analyses of Chinese Qing Dynasty Enameled Masterpieces Made Using European Ingredients/Recipes

by Philippe Colomban, Michele Gironda, Divine Vangu, Burcu Kırmızı, Bing Zhao and Vincent Cochet

Materials 2021, 14(23), 7434; https://0-doi-org.brum.beds.ac.uk/10.3390/ma14237434 - 03 Dec 2021

Cited by 16 | Viewed by 3126

Abstract

Two masterpieces of the Qing Dynasty (1644–1912 CE), one in gilded brass (incense burner) decorated with cloisonné enamels stylistically attributed to the end of the Kangxi Emperor’s reign, the other in gold (ewer offered by Napoleon III to the Empress as a birthday present), decorated with both cloisonné and painted enamels bearing the mark of the Qianlong Emperor, were non-invasively studied by optical microscopy, Raman microspectroscopy and X-ray microfluorescence spectroscopy (point measurements and mapping) implemented on-site with mobile instruments. The elemental compositions of the metal substrates and enamels are compared. XRF point measurements and mappings support the identification of the coloring phases and elements obtained by Raman microspectroscopy. Attention was paid to the white (opacifier), blue, yellow, green, and red areas. The demonstration of arsenic-based phases (e.g., lead arsenate apatite) in the blue areas of the ewer, free of manganese, proves the use of cobalt imported from Europe. The high level of potassium confirms the use of smalt as the cobalt source. On the other hand, the significant manganese level indicates the use of Asian cobalt ores for the enamels of the incense burner. The very limited use of the lead pyrochlore pigment (European Naples yellow recipes) in the yellow and soft green cloisonné enamels of the Kangxi incense burner, as well as the use of traditional Chinese recipes for other colors (white, turquoise, dark green, red), reinforces the pioneering character of this object in technical terms at the 17th–18th century turn. The low level of lead in the cloisonné enamels of the incense burner may also be related to the use of European recipes. On the contrary, the Qianlong ewer displays all the enameling techniques imported from Europe to obtain a painted decoration of exceptional quality with the use of complex lead pyrochlore pigments, with or without addition of zinc, as well as cassiterite opacifier. Full article

(This article belongs to the Special Issue Material Analysis in Cultural Heritage)

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19 pages, 4626 KiB

Open AccessArticle

Architectural Glazed Tiles Used in Ancient Chinese Screen Walls (15th–18th Century AD): Ceramic Technology, Decay Process and Conservation

by Jingyi Shen, Li Li, Ji-Peng Wang, Xiaoxi Li, Dandan Zhang, Juan Ji and Ji-Yuan Luan

Materials 2021, 14(23), 7146; https://0-doi-org.brum.beds.ac.uk/10.3390/ma14237146 - 24 Nov 2021

Cited by 5 | Viewed by 2649

Abstract

The glazed tile is an important building material used throughout the history of traditional Chinese architecture. Architectural glazed tiles used to decorate the screen walls of ancient China are studied scientifically for the first time. More than 30 glazed tile samples from the screen walls of the 15th to 18th century AD of the Hancheng Confucian Temple and Town God’s Temple in Shaanxi Province were carefully investigated using SEM–EDS and XRD. Microstructure and chemistry indicated the raw materials, the recipes and the technological choices used to produce the paste and glaze of the glazed tile samples studied. The causes for the key degradation processes of these glazed tiles used as building materials in the screen walls have also been discussed. This work has clear implications for the restoration and conservation treatments on these kinds of ancient Chinese building materials. Full article

(This article belongs to the Special Issue Material Analysis in Cultural Heritage)

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17 pages, 5324 KiB

Open AccessArticle

Archaeological and Chemical Investigation on Mortars and Bricks from a Necropolis in Braga, Northwest of Portugal

by Ana Fragata, Carla Candeias, Jorge Ribeiro, Cristina Braga, Luís Fontes, Ana Velosa and Fernando Rocha

Materials 2021, 14(21), 6290; https://0-doi-org.brum.beds.ac.uk/10.3390/ma14216290 - 22 Oct 2021

Cited by 4 | Viewed by 1460

Abstract

This investigation intends to study and characterize the mortars and bricks from walls and floors used in the funerary nucleus of the archaeological site of Dr. Gonçalo Sampaio Street (Braga, Portugal), associated with the Via XVII necropolis of the Bracara Augusta Roman city. The diversity of the funeral structures and their exceptional state of conservation make this sector of the necropolis an unprecedented case and a reference site in the archaeology of Braga, a determinant for its conservation and musealization. Nineteen mortars samples were analysed by X-ray Fluorescence. The results showed clear chemical composition differences among coating and floor mortars (CFM), masonry mortars (MM) and bricks (B) groups of samples. The chemical affinity between CFM from the V to IV centuries, CFM from the IV to V centuries, MM from brick walls (IV–V centuries), MM from stone walls (V–VII centuries) and B from the IV to V centuries samples were confirmed by statistical analyses. Their composition was distinctly related to the use of different raw materials, according to their chronological context; in mortars, according to their function in the structures; and in some samples, from contamination. Full article

(This article belongs to the Special Issue Material Analysis in Cultural Heritage)

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15 pages, 8075 KiB

Open AccessArticle

X-ray Imaging and Computed Tomography for the Identification of Geometry and Construction Elements in the Structure of Old Violins

by Mariana Domnica Stanciu, Mircea Mihălcică, Florin Dinulică, Alina Maria Nauncef, Robert Purdoiu, Radu Lăcătuș and Ghiorghe Vasile Gliga

Materials 2021, 14(20), 5926; https://0-doi-org.brum.beds.ac.uk/10.3390/ma14205926 - 09 Oct 2021

Cited by 12 | Viewed by 4014

Abstract

Numerous studies on heritage violins have shown that there are a number of factors that contribute to the acoustic quality of old violins. Among them are the geometric shape of the violin, the thickness of the tiles, the arching of the tiles, the dimensions and position of the bass bar, the size and position of the acoustic holes. Thus, the paper aims to compare the structural and constructive elements of old violins made in various famous violin workshops (Stainer, Klotz, Leeb, Babos Bela), using nondestructive and noncontact techniques based on image analysis. The violins that were studied date from 1716 to 1920, being in good condition, most of them being used by artists from the Brașov Philharmonic of Romania. In the first stage of the study, the violins were optically analyzed and scanned to identify the structure of the resonant wood, using the WinDENDRO Density 2007 program. X-ray imaging and computed tomography (CT) were also used. Combining the types of analyses, capitalizing on the expertise of violin producers and the knowledge of researchers in the field, valuable data on the geometric and constructive characteristics of old violins were extracted. Full article

(This article belongs to the Special Issue Material Analysis in Cultural Heritage)

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Review

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23 pages, 3844 KiB

Open AccessReview

Emerging Glass Industry Patterns in Late Antiquity Balkans and Beyond: New Analytical Findings on Foy 3.2 and Foy 2.1 Glass Types

by Roman V. Balvanović and Žiga Šmit

Materials 2022, 15(3), 1086; https://0-doi-org.brum.beds.ac.uk/10.3390/ma15031086 - 30 Jan 2022

Cited by 6 | Viewed by 1541

Abstract

Resolving issues posed by our paper describing the late antiquity glass from Jelica (Serbia), we performed a thorough analysis of similar glass, systematically collected from the literature. The analysis showed that Foy 3.2 type evolved gradually from a composition similar to the Roman antimony-decolorized glass to a composition approaching Foy 2.1, lasting longer (second−seventh century AD) and spreading wider than originally described, including large parts of the Balkans, France interior, Germany, and Britain. The center of its distribution seems to be the Balkans and Italy. During the sixth century, Foy 3.2 glasses in the Balkans showed a significant increase of average MgO concentration compared to the earlier period and Foy 3.2 glasses outside the Balkans, implying different sand quarries and perhaps different trade routes for its imports. Recycling criteria for Foy 3.2 glass has been established. Similarly, 125 high-iron Foy 2.1 glasses are selected from the literature. They cluster within two groups regarding iron concentrations, which we term high iron (HI) and very high iron (VHI) Foy 2.1. In addition, there is a low lime subgroup of the VHI group, termed VHILL. The paper offers two possible explanations for the elevated iron, color branding, and different silica sources. High-iron glasses seem relatively evenly spread across the entire Mediterranean and its interior, representing, on average, around a quarter of the local Foy 2.1 assemblages. The percentages of high-iron samples are almost double in manufactured glass compared to raw glass, suggesting that the addition of iron was happening in the secondary workshops, i.e., for color branding. Among the manufactured glass, the proportions were higher in glassware than in windowpane glass. To capture the changing sand exploitation conditions, we propose the term “generic composition/type” or “(geochemical) class”. Full article

(This article belongs to the Special Issue Material Analysis in Cultural Heritage)

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