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Materials in Cultural Heritage: Analysis, Testing, and Preservation

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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 May 2025) | Viewed by 10074

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Prof. Dr. Žiga Šmit

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Guest Editor

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,

The achievements of past generations are a valuable tangible or intangible memory for the present, as we admire and learn from the actions of the past. In short, we call this memory cultural heritage, which is both material and immaterial. It is, however, the material heritage that is subject to constant deterioration and decay; therefore, it requires special care for its preservation. On the other hand, some historical facts about the objects’ production, usage and distribution are hidden within the objects themselves and not well understood, so we are hoping to learn more about them by applying specific analytical methods, which may reveal unseen connections between objects and their use, regions, and cultural groups. Today, several researchers devote their efforts to the studies of cultural heritage objects, both in terms of their preservation (or conservation) and investigation. Their endeavours traditionally bear the name of archaeometry and conservation science, with both terms recently being supplemented by the term heritage science.

A year ago, we edited a Special Issue of Materials entitled “Material Analysis in Cultural Heritage”. Due to increased interest in the field, we are now calling for the second part under an updated name “Materials in Cultural Heritage: Analysis, Testing, and Preservation”, with the following key points:

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: archaeological and historic glass, metals, pigments and lithic materials;
Experimental archaeology, i.e., reconstruction of ancient techniques and materials.

You are invited to submit a manuscript.

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

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

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Keywords

cultural heritage materials
archaeological materials
ancient techniques and materials
analytical techniques

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Published Papers (11 papers)

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Research

23 pages, 10361 KiB

Open AccessArticle

Analysis of the Material and Coating of the Nameplate of Vila D. Bosco in Macau

by Liang Zheng, Jianyi Zheng, Xiyue He and Yile Chen

Materials 2025, 18(10), 2190; https://doi.org/10.3390/ma18102190 - 9 May 2025

Viewed by 339

Abstract

This study focuses on the nameplate of Vila D. Bosco, a modern building in Macau from the time of Portuguese rule, and looks at the types of metal materials and surface coatings used, as well as how they corrode due to the tropical marine climate affecting the building’s metal parts. The study uses different techniques, such as X-ray fluorescence spectroscopy (XRF), scanning electron microscopy/energy dispersive spectroscopy (SEM-EDS), X-ray diffraction (XRD), attenuated total internal reflectance Fourier transform infrared spectroscopy (ATR-FTIR), and cross-sectional microscopic analysis, to carefully look at the metal, corrosion products, and coating of the nameplate. The results show that (1) the nameplate matrix is a resulfurized steel with a high sulfur content (Fe up to 97.3% and S up to 1.98%), and the sulfur element is evenly distributed inside, which is one of the internal factors that induce corrosion. (2) Rust is composed of polycrystalline iron oxides such as goethite (α-FeOOH), hematite (α-Fe₂O₃), and magnetite (Fe₃O₄) and has typical characteristics of atmospheric oxidation. (3) The white and yellow-green coatings on the nameplate are oil-modified alkyd resin paints, and the color pigments are TiO₂, PbCrO₄, etc. The surface layer of the letters is protected by a polyvinyl alcohol layer. The paint application process leads to differences in the thickness of the paint in different regions, which directly affects the anti-rust performance. The study reveals the deterioration mechanism of resulfurized steel components in a subtropical polluted environment and puts forward repair suggestions that consider both material compatibility and reversibility, providing a reference for the protection practice of modern and contemporary architectural metal heritage in Macau and even in similar geographical environments. Full article

(This article belongs to the Special Issue Materials in Cultural Heritage: Analysis, Testing, and Preservation)

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25 pages, 6263 KiB

Open AccessArticle

Analysis of Late Antique and Medieval Glass from Koper (Capodistria, SI): Insights into Glass Consumption and Production at the Turn of the First Millennium CE

by Žiga Šmit and Tina Milavec

Materials 2025, 18(9), 2135; https://doi.org/10.3390/ma18092135 - 6 May 2025

Viewed by 274

Abstract

A series (n = 22) of glasses from the site Kapucinski vrt (garden of the Capuchin monastery, 5th–17th c. CE) in Koper (Capodistria), a port town in the northern Adriatic, was measured using a combined PIXE and PIGE method. Koper has been continuously populated since the late Roman period, with a rich medieval history, thus offering an opportunity to study Early Medieval glass. Stemmed goblet fragments, in the original publication dated between the 6th–9th centuries CE, and several other vessel types (beakers and flasks or bottles and lamps) were selected for analysis. The measurements were expected to show the trends in glass production and consumption from Late Antiquity until the Middle Ages, notably the transition between natron to plant ash glass and the supply of fresh glass. Among the set of 22 glass vessel fragments, both natron and plant ash glass were identified. For finer classification, we relied on a newly developed method of Euclidean distances with respect to major concentrations. Natron glass of the types Foy 2.1 (9 examples), Magby (2 examples), and Levantine I (Apollonia; 2 examples) was found. Two glasses remain undetermined but testify to an Egyptian origin. Most natron glasses show signs of recycling. Among the three unrecycled glasses (about 20% of the whole set), there are two examples of Levantine glass and a Magby glass lamp; this may indicate a modest supply of fresh glass during the period. Plant ash glass may be attributed to the Early or High Middle Ages, exploiting the purified alkalis of the Levantine coasts (known as alume catino in later Venetian glassmaking), and the admixture of impurities in the siliceous sands suggests the circulation and consumption of glass that was produced and traded in the eastern Mediterranean since the 10th century CE. Full article

(This article belongs to the Special Issue Materials in Cultural Heritage: Analysis, Testing, and Preservation)

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26 pages, 8874 KiB

Open AccessArticle

Radiocarbon Dating of Mortar Fragments from the Fresco of a Romanian Monastery: A Field Study

by Marioara Abrudeanu, Corina Anca Simion, Adriana Elena Valcea, Maria Valentina Ilie, Elena Alexandra Ispas, Maria Loredana Marin, Dragos Alexandru Mirea, Dan Cristian Olteanu, Cristian Manailescu, Alexandru Razvan Petre, Denis Aurelian Negrea, Sorin Georgian Moga, Izabela Maris, Dorin Grecu, Gheorghe Garbea, Flavio Nicolae Finta and Mircea Ionut Petrescu

Materials 2025, 18(5), 1149; https://doi.org/10.3390/ma18051149 - 4 Mar 2025

Viewed by 621

Abstract

The stone Ensemble from Corbii de Piatrǎ Romania arouses a continuous scientific interest, with the final goal being to obtain an exhaustive and multidisciplinary package of results that will become the support of an extensive restoration project. The cave painting stands out as the most important and most affected by the advanced degradation among the historical monuments in Romania. This article provides for the first time a radiocarbon dating of the first forms of painting by establishing the age of the mortar/plaster used as a pictorial support. Being a very complex context from the point of view of the type of datable material and the disappearance over time through degradation of other elements that would ensure a simpler and more reliable radiocarbon dating (such as the straws used to form the material), it was necessary to use a multidisciplinary approach for the selection of samples and for supporting the radiocarbon results. The set of analyses consisted of visualization techniques through microscopy and compositional analysis, providing information on the similarities/differences between the samples, the degradation mechanisms/impurities and the quality of the calcium carbonate dated by the Accelerator Mass Spectrometry (AMS) technique. The results supported each other, ensured the selection of reliable radiocarbon data and established the most probable moment of the early interventions, namely the two phases corresponding to the 14th century. Full article

(This article belongs to the Special Issue Materials in Cultural Heritage: Analysis, Testing, and Preservation)

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13 pages, 1816 KiB

Open AccessArticle

Non-Destructive Ellipsometric Analysis of the Refractive Index of Historical Enamels

by Teresa Palomar, Trinitat Pradell and Jadra Mosa

Materials 2025, 18(5), 1137; https://doi.org/10.3390/ma18051137 - 3 Mar 2025

Viewed by 508

Abstract

The refractive index is an important parameter for the restoration of historical cultural heritage and for non-destructive optical techniques. In this study, different mathematical models for lead glasses were assessed in order to analyze their feasibility to calculate the theoretical refractive index of the historical enamels in stained-glass windows. The models selected were those specifically developed for lead glasses: the Appen method (1949), the Fanderlik and Skrivan model (1972), and the Bonetti and Salvagno method (1983). The results of the mathematical methods were compared with the real values analyzed via ellipsometry. The historical enamels were determined on non-prepared samples, taking into account the Cauchy model in order to avoid damaging the historical pieces. We show that the measured refractive indices of the historical enamels (1.59–1.66) are higher than the values of the lead glasses in the literature (1.55–1.57). The PbO and B₂O₃ were the compounds that most influenced the value of the refractive index; nevertheless, the presence of metallic elements increased their value compared to pure lead glasses. In addition, the presence of a thin layer of grisaille on the historical enamels and the formation of alteration layers could also modify the real value of the refractive index. As far as theoretical calculations are concerned, the mathematical model of Bonetti and Salvagno (1983) seems to be the most accurate model for this material, with errors < 0.04 units. None of the three models work for glasses with >60% PbO, which is not common in cultural heritage. Full article

(This article belongs to the Special Issue Materials in Cultural Heritage: Analysis, Testing, and Preservation)

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11 pages, 6234 KiB

Open AccessArticle

Where Did Vessels Come from? A Study of Pottery Provenance from the Site of Velika Humska Čuka, Serbia

by Maja Gajić-Kvaščev, Ognjen Mladenović, Petar Milojević and Aleksandar Bulatović

Materials 2025, 18(5), 1083; https://doi.org/10.3390/ma18051083 - 28 Feb 2025

Viewed by 513

Abstract

The archaeological materials from the Velika Humska Čuka site on the northern fringe of the Niš Basin in southeastern Serbia were analyzed to reveal the provenance of ceramics and other artifacts. This study focused on the elemental analysis of 61 samples, including local clay pits, potsherds, and whole vessels. Samples were chosen based on stylistic and typological characteristics to distinguish local and “foreign” pottery. Elemental analysis was conducted using energy-dispersive X-ray fluorescence (EDXRF) spectrometry, complemented by principal component analysis (PCA) for data interpretation. Results indicated that the majority of pottery samples, over 80%, were produced using local clay from deposits near the site. However, approximately 20% of the analyzed vessels were made using clay from deposits near the Bubanj site, 8 km south of Velika Humska Čuka. A vessel on a hollow high foot combining stylistic elements of the Bubanj-Hum I group and Early Eneolithic Pannonian groups was made of clay not sourced from any identified local deposits, suggesting its non-local origin. While the predominance of local materials suggests self-sufficient production, the use of non-local clays and stylistic influences highlights long-distance connections and exchanges. The study emphasizes the importance of Velika Humska Čuka in understanding the development of ceramic traditions and the cultural dynamics of the Early Eneolithic in the Central Balkans. Full article

(This article belongs to the Special Issue Materials in Cultural Heritage: Analysis, Testing, and Preservation)

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16 pages, 887 KiB

Open AccessArticle

Integrating Attenuated Total Reflectance–Fourier Transform Infrared Spectroscopy and Multidetector Computed Tomography for Analysis of Heat-Induced Changes in Bone

by Tamara Leskovar, Fabio Cavalli, Lea Legan, Dario Innocenti, Polonca Ropret and Matija Črešnar

Materials 2025, 18(4), 742; https://doi.org/10.3390/ma18040742 - 7 Feb 2025

Cited by 1 | Viewed by 752

Abstract

Charred and burned human and animal skeletal remains are frequently found in archaeological records and can also be subjects of forensic investigations. Heat exposure causes specific changes to the physical and chemical characteristics of these remains, offering valuable insights into their taphonomic history. This research combines the commonly used ATR-FTIR (Attenuated Total Reflectance–Fourier Transform Infrared) spectroscopy with the rarely utilised density measurements obtained from Multidetector CT (Computed Tomography) to investigate changes in defleshed bovine cortical bone exposed to different temperatures for varying durations. The inclusion of density measurements is significant because Multidetector CT analysis is non-destructive and can be valuable when remains cannot be removed from their burial context (e.g., urn) or cannot be damaged. The results indicate complex changes in both organic and inorganic components, affecting crystallinity and density. Lower temperatures primarily affect organic matter, while higher temperatures induce significant changes in the mineral lattice and phase transitions. The transformation from β-tricalcium phosphate to α-tricalcium phosphate at high temperatures likely impacts the bone’s crystallinity and density. Bone density measured by CT scans provided additional information that complemented the interpretations of FTIR spectroscopy. While CT scans offer important data for planning non-destructive analyses of remains, they present only one layer of information. Therefore, CT scans need to be combined with other techniques to provide comprehensive interpretations of the changes occurring in the bone. Further research is needed on density measurements and other potentially non-destructive analyses to fully unlock the potential of Multidetector CT analyses. Full article

(This article belongs to the Special Issue Materials in Cultural Heritage: Analysis, Testing, and Preservation)

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21 pages, 3260 KiB

Open AccessEditor’s ChoiceArticle

Amber “Alchemy”: Recreating and Investigating Yellow Glass Formulations

by Catarina Reis Santos, Andreia Ruivo, Ana Carneiro, João Pedro Veiga, Teresa Palomar and Inês Coutinho

Materials 2024, 17(23), 5699; https://doi.org/10.3390/ma17235699 - 21 Nov 2024

Viewed by 1010

Abstract

Amber glass has been produced since at least the 6th century BC. Its value derives from its ability to mimic natural amber and, later, from its ultraviolet filtering properties. Until the 19th century, amber glass was widely used for the storage of food and medicines because its protective properties had been empirically recognized. This study investigates historical methods of amber glass production by using glass recipes from four Portuguese arcana (1793–1975) and focusing on Fe-S and Fe-Mn chromophores. Five recipes were reproduced under controlled laboratory conditions, resulting in 21 experiments. Of these, only 10 produced amber glasses were with different shades. Chemical compositions were analysed by WDXRF, while DSC and dilatometry were used to assess thermal properties. Vickers hardness tests and UV–visible absorption spectroscopy provided insight into mechanical strength and chromophore presence. The study found that FeS amber glass was more difficult to produce than Fe-Mn amber glass, given the complex variables involved in the former, such as SO₃ volatility affecting the final product. Reproduction of historical recipes showed that, even without modern chemical knowledge, historical glassmakers developed practical, empirical methods for making amber glass. These findings contribute to a broader understanding of glass conservation and highlight the importance of historical glass recipes for the interpretation and conservation of glass objects. Full article

(This article belongs to the Special Issue Materials in Cultural Heritage: Analysis, Testing, and Preservation)

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23 pages, 15467 KiB

Open AccessArticle

Characterization and Making Techniques of Calcareous Construction Materials for Phaya Thon Zu Temple in Bagan Historical Area, Myanmar

by Hye Ri Yang, Gyu Hye Lee, Dong Min Kim and Chan Hee Lee

Materials 2024, 17(17), 4294; https://doi.org/10.3390/ma17174294 - 30 Aug 2024

Viewed by 960

Abstract

The calcareous materials used in constructing the Phaya Thon Zu temple at the Bagan historical sites in Myanmar are mortars, plasters, and stuccos. Among them, the mortars and plasters are a mixture of original and new materials used for recent conservation treatments. In this study, the making techniques were examined through analysis of calcareous materials by production period. All calcareous materials have a mineral composition similar to soil, except calcite. Stuccos have the most refined aggregates, homogeneous particle size, and the highest lime and organic contents. They were designed to improve ease of carving and weathering resistance, considering the unique characteristics of the stuccos. Because all calcareous materials were mixed with soil, the origin of the clay materials was analyzed. It was concluded that the mortars were produced by mixing clay and sandy soil, and the original mortars showed characteristics similar to soil. It is highly possible that sandy soil from around the Htillominlo temple was used to produce new plasters, and it is estimated that a mixture of clay soil was used for the original plasters and stuccos. A clear provenance interpretation of the original and raw materials used for each construction and the mixing ratio of clay materials need to be discussed through experiments, along with the estimated provenance area of the raw calcareous materials. Full article

(This article belongs to the Special Issue Materials in Cultural Heritage: Analysis, Testing, and Preservation)

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12 pages, 5787 KiB

Open AccessArticle

Comparison of Quantitative and Qualitative EDXRF Analysis for Provenance Study of Archaeological Ceramics

by Maja Gajic-Kvascev, Velibor Andric, Radmila Jancic-Heinemann, Ognjen Mladenovic and Aleksandar Bulatovic

Materials 2024, 17(15), 3725; https://doi.org/10.3390/ma17153725 - 27 Jul 2024

Cited by 2 | Viewed by 1068

Abstract

The most common scientific analysis of archaeological ceramics aims to determine the raw material source and/or production technology. Scientists and archaeologists widely use XRF-based techniques as a tool in a provenance study. After conducting XRF analysis, the results are often analyzed using multivariate analysis in addition to interpretation and conclusions. Various multivariate techniques have already been applied in archaeological ceramics provenance studies to reveal different raw material sources, identify imported pieces, or determine different production recipes. This study aims to evaluate the results of multivariate analysis in the provenance study of ceramics that belong to three cultures that settled in the same area during various prehistoric periods. Portable energy-dispersive X-ray fluorescence spectrometry (pEDXRF) was used to determine the elemental composition of the ceramic material. The ceramic material was prepared in two different ways. The ceramic body material was ground into powder, homogenized, and then pressed into tablets. After that, the same fragments are polished in suitable places. Quantitative and qualitative analyses were performed on the tablets and polished pieces. The results were subjected to both unsupervised and supervised multivariate analysis. Based on the results, it was concluded that qualitative analysis of the well-prepared shards’ surface using EDXRF spectrometry could be utilized in provenance studies, even when the ceramic assemblages were made of similar raw materials. Full article

(This article belongs to the Special Issue Materials in Cultural Heritage: Analysis, Testing, and Preservation)

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21 pages, 4863 KiB

Open AccessEditor’s ChoiceArticle

Antifungal Hybrid Graphene–Transition-Metal Dichalcogenides Aerogels with an Ionic Liquid Additive as Innovative Absorbers for Preventive Conservation of Cultural Heritage

by George Gorgolis, Maria Kotsidi, Elena Messina, Valentina Mazzurco Miritana, Gabriella Di Carlo, Elsa Lesaria Nhuch, Clarissa Martins Leal Schrekker, Jeniffer Alves Cuty, Henri Stephan Schrekker, George Paterakis, Charalampos Androulidakis, Nikos Koutroumanis and Costas Galiotis

Materials 2024, 17(13), 3174; https://doi.org/10.3390/ma17133174 - 28 Jun 2024

Cited by 3 | Viewed by 1634

Abstract

The use and integration of novel materials are increasingly becoming vital tools in the field of preventive conservation of cultural heritage. Chemical factors, such as volatile organic compounds (VOCs), but also environmental factors such as high relative humidity, can lead to degradation, oxidation, yellowing, and fading of the works of art. To prevent these phenomena, highly porous materials have been developed for the absorption of VOCs and for controlling the relative humidity. In this work, graphene and transition-metal dichalcogenides (TMDs) were combined to create three-dimensional aerogels that absorb certain harmful substances. More specifically, the addition of the TMDs molybdenum disulfide and tungsten disulfide in such macrostructures led to the selective absorption of ammonia. Moreover, the addition of the ionic liquid 1-hexadecyl-3-methylimidazolium chloride promoted higher rates of VOCs absorption and anti-fungal activity against the fungus Aspergillus niger. These two-dimensional materials outperform benchmark porous absorbers in the absorption of all the examined VOCs, such as ammonia, formic acid, acetic acid, formaldehyde, and acetaldehyde. Consequently, they can be used by museums, galleries, or even storage places for the perpetual protection of works of art. Full article

(This article belongs to the Special Issue Materials in Cultural Heritage: Analysis, Testing, and Preservation)

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14 pages, 3390 KiB

Open AccessArticle

Analysis of the Surface of Historic Fabric from the Auschwitz-Birkenau State Museum after Treatment with Ethanol Mist Used to Eliminate Microorganisms Harmful to Human Health

by Anna Wawrzyk, Janina Poskrobko, Krystyna Guzińska, Dorota Kaźmierczak, Aleksandra Papis, Nel Jastrzębiowska, Natalia Uroda, Maria Szymankiewicz, Dagmara Zeljaś, Iga Wawrzyk-Bochenek and Sławomir Wilczyński

Materials 2024, 17(10), 2323; https://doi.org/10.3390/ma17102323 - 14 May 2024

Cited by 2 | Viewed by 1127

Abstract

Aim: the aim of the work was to present the changes occurring on the model and historical cotton surface of cotton resulting from disinfection with 90% ethanol mist. Materials and methods: Samples of historical materials consisted of fabric elements from suitcases stored in A-BSM. A mist of 90% ethanol was applied for 15 s at a distance of 16 cm from the surface. The spectra of cotton samples before and after ethanol application were recorded using Fourier transform infrared spectroscopy (FTIR-ATR). Analyses of the surface layers were performed using X-ray photoelectron spectroscopy (XPS). Results: the decontamination performed did not show any significant differences in the chemical composition and surface structure of cotton before and after the use of 90% ethanol mist. Conclusions: Ethanol mist, which eliminates microorganisms from the historical surface, does not cause significant changes to the surface of historical objects. Full article

(This article belongs to the Special Issue Materials in Cultural Heritage: Analysis, Testing, and Preservation)

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