New Materials in The Conservation of Mural Paintings to Obtain High Durability, Tomb of Keamun TT 93, Luxor, Egypt

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New Materials in The Conservation of Mural Paintings to Obtain High Durability, Tomb of Keamun TT 93, Luxor, Egypt

https://doi.org/10.21203/rs.3.rs-3269996/v1

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The aim of this research to study the treatment of mural painting at the tomb of Kenamun TT93 back to 18th Dynasty back to New Kingdom (c. 1550-1069 BC.), in the Theban Necropolis, on the west bank of the Nile. In this study the surface of deteriorated mural paintings were investigated using PLM (BMM), TEM investigation, XRD analysis, FTIR spectroscopy, and SEM-EDX. To our knowledge, it is the first report on the mixture of the ethyl silicate and the Egg shell Nanoparticles application of mixture for the treatment of deteriorated mural painting surfaces in Tomb of Kenamun TT93.The samples were collected from Fragment of wall painting, painted with depiction of two women, Tomb of Keamun (TT93). The results of obtained show that the structures fragment of wall painting consist of three layers from the top to bottom: yellow pigment, fine plaster, coarse plaster which contains composed of quartz, clay minerals, iron oxides, and organic fibers. The selection of these samples was due to historical importance, which is directly related to ancient Egyptian heritage.

Mural painting

Luxor

Conservation

Cracks

Egg shell Nanoparticles

In the Sheikh Abd el-Qurna, in the Theban Necropolis, on the west bank of the Nile, tomb of Kenamun TT93 back to 18th Dynasty. More than three hundred tombs can be found there, all belonging to New Kingdom (c. 1550 − 1069 BC.

1.1. The Tomb of Kenamun - TT93

The tomb of Kenamun TT93 is located in Ancient Thebes. It is at the top of the mountain where we call today the tombs of the Nobles, at Sheikh Abd el-Qurna, across the river Nile from the city of Luxor. This palace-like tomb, that is approximately 3.400 years old, is full of wall paintings. TT93 stands for Theban tomb number 93. A designation given to it in much more recent times to record and locate many tombs of many sizes, from very small to large tombs in Luxor (the ancient Thebes), built in antiquity into the bedrock by digging and carving out stone from the mountain to sculpt the desired architectural design into it. The tomb has never been thoroughly excavated or studied, but has been visited by scholars in the XIXth and XXth century. The famous Jean-François Champollion (the first to decipher Egyptian hieroglyphs) and Ippolito Rossellini (the founder of Italian Egyptology) made a 2 year French-Tuscan expedition together to Egypt in 1828 and they visited the tomb of Kenamun. In the early nineteenth century, Champollion, Lepsius, Wilkinson and Prisse d'Avennes visited the tomb, but until the Metropolitan Museum of Art published the tomb of Ken-Amun at Thebes in the late 1920s, which details its exploration and documents its contents, it was largely neglected. [1–5]. Figure (1).

Figure (1) a. Showing the location of the tomb of Kenamun - TT93 in Luxor

(https://www.kenamun.com/gallery-miscellaneous) b Plan of the tomb (https://en.wikipedia.org/wiki/TT93), c The main entrance of the Kenamun tomb - TT93

1.2. The geological structure of the Theban Necropolis

A geological study finds that the west bank of Luxor consists of three main formations, which are > 350 m thick: 1) The base is tarawan chalk a; 2) The middle is Esna shale ; and 3) The top is Thebes limestone.

In the Theban Mountains, which rise approximately 462 meters above sea level, marine limestone (lower Eocene) and marls more than 350 meters thick dominate. Noble’s tombs were cut into the bedrock of the Theban Mountains. In the tombs of the area, a characteristic Esna shale formation can be found sporadically with a thickness of about 55 meters. Geology of the studied area plays an important role in defining the conservation state of the tombs. The Theban Mountains are mostly composed of clay minerals and carbonates, with small amounts of quartz, gypsum, halite, and anhydrite. When clay minerals and soluble salts are present in the geological structure, deterioration is more effective. [6–10].

Stone quality at Thebes is poor, so most tomb chapels were plastered and painted rather than decorated with reliefs. The tomb of Kenamun - TT93 suffering from different weathering forms such as cracks, strength loss and detachment of plaster due to the harsh weather conditions in Luxor, the wall paintings are exposed to different the high value of temperatures (41–50°C) in summer and temperatures (7°C) in winter. [9–15].

Based on the visual observations of the tomb of Kenamun - TT93, many vertical and horizontal cracks were observed in the wall paintings, as well as crack networks in the mural painting surfaces due to deterioration factors. Figure (2,3).

Figure (2) a. ,b ,c. showing the horizontal and vertical cracks, gaps, exfoliation and the fragment plaster, c. showing the crack networks in the mural painting surfaces due to deterioration factors.

Figure (3) a. showing Fragment of wall painting, painted with depiction of two women, Tomb of Keamun (TT93) b. c. Mapping of the mural painting condition and place the crack via Auto CAD

3.1. Materials

Sample was chosen from damaged of the wall painting including yellow color was collected to characterize the wall paintings at the tomb of Keamun (TT93) to provide the information about the cross section of the paint layers of the Fragment of wall painting. The Number of the Epoxy and the hardener is 27–751, sizes of Sandpaper (800: 4000) were used to preparation of the samples.

3.2. Samples Preparation:

The samples to be used for Cross-Section were divided into small pieces, then embedded in epoxy after the completely drying the epoxy, the samples were polished by using sandpaper different sizes with wet-type sandpaper to get smooth. Figure (4).

Figure (4) a. Photomicrograph of cross-section image showing the structures of mud mortar mainly clay minerals, lime, sand, aggregates and animals dung addition to chopped straw as binding cementing materials. under normal light under PLM (BMM), b under UV light

3.3. Characterization of the Egg shell Nanoparticles

Two treatment products were applied to injection the cracks: 1) the Egg shell Nanoparticles product); 2) Ethyle silicate 3% that can be used to injection the crack networks in the mural painting surfaces. To our knowledge, it is the first report on the application of Egg shell Nanoparticles for the injection of cracks mural painting surfaces

Eggshell is a natural bio ceramic composite that has a unique chemical make–up of inorganic and organic compounds. It consists of an inorganic shell and an organic membrane. The shell together with its membrane weighs approximately 11% of the egg weight. The inorganic constituent of eggshells is mainly calcium carbonates (95% in the form of calcite), whereas its organic compounds are a matrix of proteins, glycoprotein, proteoglycan, and type X collagen sulphated polysaccharides (5%) [16–18]. Owing to this unique chemical composition, eggshell has extensively gained attention among researchers for its medical and dental benefits. For example, Khandelwal and Prakash [19]. demonstrated how calcium carbonate derived from eggshells could be used to produce hydroxyapatite, which is mainly used in bone and dental treatments. Abdulrahman, Tijani, Mohammed, Yusuf, Jibrin and Mohammed [20]. alleged that eggshells based hydroxyapatite and nanohydroxyapatite could reduce the cost of treatment in bone repair or replacement

3.4. Preparation Method of the Egg shell Nanoparticles:

The Chicken Egg Shell Powder was prepared by the calcination protocol given by World Property Intellectual organization (WO/2004/105912: Method of Producing egg shell powder) [21]. Chicken Egg Shell contains about 95% of calcium carbonate which on conversion to basic calcium oxide due to calcination is responsible for an increase in alkalinity [22]. Twelve chicken eggs used were cleaned with distilled water and kept in hot boiling water for 10 mins at 100°C to facilitate the removal of membranes. The egg shells were crushed and powdered to small particles with sterile mortar and pestle. The tiny, crushed particles obtained were then kept in a muffle furnace (Ney craft Model JFF 2000) at 1200°C to make sure the resulting powder is pathogen free. Then the dried powder was milled by using milled by ball mill machine (planetary-ball-mill-pm-400) for 10h, speed 350rpm and 3min intervals.

3.5. Application of Nano-Composite

The Nano mixture preparation using the sonication technique by dispersing 20 gm wt% of Egg shell Nanoparticles powder (average size 50 nm) in 1000 mL of ethanol for 30 min using an ultrasonic mixture and magnetic stirrer. The Egg shell Nanoparticles mixed with Ethyle silicate in 1:1 ratio. After that use an ultrasonic mixture and magnetic stirrer for 25 min for homogeneous textures.

3.6. Analyses and investigations

3.6.1. TEM investigation (Morphological study):

Size & Shape: The HR-TEM is JOEL JEM-2100 operating at 200 kV equipped with Gatan digital camera Erlangshen ES500. Figure (5)

Figure (5) a.b. shows the TEM images of the Eggshells nanoparticles at difference magnification.

3.6..2 XRD analysis

X-ray diffraction pattern has been performed using XPERT-PRO Powder Diffractometer system, with 2 theta (20ᴼ − 80ᴼ), with Minimum step size 2Theta: 0.001, and at wavelength (Kα) = 1.54614ᴼ. Figure (6).

Figure (6) Shows the XRD pattern of egg shell after thermal treatment at 1200^o C and milling.

3.6.3. FTIR spectroscopy:

FT-IR vertex 70 RAM II, Bruker Spectometer was used to measurement of nano eggshells

Figure (7).

Figure (7) shows the FTIR spectrum of nano eggshells

4.1. PLM Observation (BMM):

The cross-section is useful for the investigation of materials. examination by PLM was used to examine Fragment of wall painting identified three layers. The structures fragment of wall decoration three layers from the top to bottom: yellow pigment, fine plaster, coarse plaster. The cross-section study revealed that the sample composed essentially of three layers from the top to bottom: yellow pigment, fine plaster, coarse plaster. Also, the cross-section study revealed that the studied sample is composed of quartz, clay minerals, iron oxides, and organic fibers. PLM microscope investigation revealed that the yellow pigment formed of very homogeneous and fine grains has many vertical and horizontal cracks and had a loos surface as a result of shrinkage of the clay minerals in the preparatory layers, cracks appear in the painting layer. This suggested that yellow pigment was produced using iron oxides. It also showed that the fine plaster layer composed formed of homogenous fine grains. [6–8]. Figure (8,9).

Figure (8) a, b. Show Fragment of wall decoration, painted with depiction of two women, Tomb of Keamun (TT93) It is return back to Egypt as a gift from the Clos Foundation, Spain, 0n 30/1/2009 Luxor

Figure (9) a, b. Photomicrograph of cross-section image showing the structures fragment of wall decoration three layers from the top to bottom: yellow pigment, fine plaster, coarse plaster, under PLM (BMM). (b) Mapping of the cross-section via Auto CAD

4.2. Observation and Analysis by SEM-EDX:

The structure investigation of fragment of wall decoration SEM images Fig. [9] showed the cross-section observation identified three layers was applied on the surface of the wall. SEM investigation showed the structures fragment of wall composed essentially of three layers from the bottom to top: coarse plaster, fine plaster and yellow pigment. the coarse plaster showed clay minerals, quartz, and straw, A bonding material was added to the mud mixture. Furthermore it showed the deterioration, such as granular disintegration, cracking, Additionally, these layers are also weak in the internal structure, which leads to many cracks. Figure (10, a).

4.3. EDX Analysis:

Fragment of wall decoration of The Tomb of Kenamun (TT93):

The coarse and fine plaster of the fragment consist of calcite (Ca) calcium carbonate CaCO₃, sulfate (S) sulfate dihydrate Ca SO₄.2H₂O (gypsum), quartz (Si), aluminium (Al), and Magnesium (Mg) clay minerals where the high beaks of O, Al, and Si, Fig. 10. [c]. The ancient Egyptian artist used yellow pigment (goethite) extensively from pre dynastic to the Roman period and used to paint the skin of women in ancient Egypt. the yellow pigment (goethite) was around oasis of the western desert and Aswan [23–24].

The yellow pigment based mainly on (Fe) (probably goethite) α-FeO (OH). The spectrum related to iron indicates the presence of iron oxide (goethite) EDX analysis showed a mixture of Fe and As-based pigments, probably orpiment As₂ S₃ mixed with goethite. Figure (10,b,c).

Figure (10) a, SEM image of showing three layers of the structures fragment of wall decoration

; b.EDX analysis showing yellow pigment c. EDX analysis showing coarse and fine plaster.

As a result of the above studies, the studied wall paintings were evaluated using the following criteria.

5.1. Pre-consolidation

The first step was to apply temporary strips of tissue paper with ethyl silicate 3%, in order to prevent weak parts of the plaster from collapsing.

5.2. Mechanical cleaning

After the mural paintings had been pre-consolidated, surface deposits were carefully removed. where, the remove dust from mural paintings using an air pump and soft brushes.

5.3. Re-adhesion of detachment and cracks

The goal of this injections is to prevent the remaining parts of mural paintings and conserve it from collapsing in the long term. To treatment the crack network and flaking paints of the mural painting, we injected 1 syringe of alcohol in the injection hole in order to prepare the cracks for the injection of the nano composite, Starting the injection process from the lower to the higher level, after that, we injected the nano composite of Egg shell Nanoparticles and Ethyle silicate 3% that can be used to injection the crack networks in the surfaces of mural painting. in the voids between the layer of painting using a thin syringe. Figure (11:15).

Figure (11) showing the experimental sample that were prepared with the same characteristics as the mural paintings in the tomb of Keamun (TT93)

Figure (12) a,b showing the horizontal and vertical cracks before treatment

Figure (13) a b showing the cracks injection

Figure (14) a b,c,d. showing the horizontal and vertical cracks after treatment

Figure (15) a b,c showing the Preparation of the Egg shell Nanoparticles by vortex (a) and ultra-sonic

(b) and the experimental sample

5.4. Nano-Composite Result:

The surface morphology of the mural painting samples was investigation using SEM (JEOL/JSM- 5500LV) and samples were observed at the South Valley University Central Laboratory in Qena, Egypt. Different changes in the sample were observed in the SEM images before and after consolidation. In consolidation samples, ethyl silicate and the Egg shell Nanoparticles are mixed, while granular disintegration is observed before consolidation, figure (16,17).

Figure (16) ) a b,c Shows SEM images of untreated samples of painted layer

Figure (17) ) a : h Shows SEM images of treated samples of painted layer by ethyl silicate and the Egg shell Nanoparticles are mixed, images d, f shows good distribution of the Egg shell Nanoparticles

Microscopic investigation and analytical study indicate that the ancient Egyptian artist prepared the mural paintings using traditional techniques. The structures fragment of wall painting consist of three layers from the top to bottom: yellow pigment, fine plaster, coarse plaster. Due to the harsh weather conditions in Luxor, Kenamun's tomb - TT93 has different forms of weathering such as cracks, strength losses, and detachment of plaster. Consolidating and filling gaps and cracks posed the greatest challenge to treating the studied mural paintings because of their fragility. The results of experimental study showed that the mixture of the Egg shell Nanoparticles and Ethyle silicate 3% that can be used to injection the crack networks in the mural painting surfaces .This mixture is highly effective at consolidating cracks and the appearance of the treated surfaces was preserved and not any changes. On the other hand, the mixture of Egg shell Nanoparticles and Ethyle silicate 3% suitable for treatment of cracks and more matching in color. The conservation steps were successfully carried out to consolidate the cracks, which include multiple processes. The first step was to apply temporary strips of tissue paper with ethyl silicate 3%, in order to prevent weak parts of the plaster from collapsing. The next step was mechanical cleaning had been pre-consolidated, surface deposits were carefully removed. The final step was Re-adhesion of detachment and cracks by injection of the nano composite, Starting the injection from the lower to the higher level, injection the crack networks in the surfaces of mural painting.

Availability of data and materials

All data generated or analyzed during this study are included in this published article and its supplementary. information files

Competing interests

The authors declare that they have no competing interests

Funding

Open access funding provided by The Science, Technology & Innovation Funding Authority (STDF) in cooperation with The Egyptian Knowledge Bank (EKB). This research received no funding from any governmental or non- governmental agencies. Any necessary funding was made by the authors themselves.

Authors' contributions

"Ezz A. Orabi tested the mural painting samples before and after treatment. and Ahmed Sallam collected historical samples, prepared the mural painting samples, applied the Egg shell Nanoparticles and ethyl silicate to the mural painting samples, Both authors read and approved the final manuscript"

Acknowledgements

The Authors would like to thank Mr. Hazem M. , Central Lab. at SVU, Qena ,Egypt, who investigated the treated samples by Scanning Electron Microscope.

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No competing interests reported.

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New Materials in The Conservation of Mural Paintings to Obtain High Durability, Tomb of Keamun TT 93, Luxor, Egypt

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Abstract

Figures

1. Introduction

1.1. The Tomb of Kenamun - TT93

1.2. The geological structure of the Theban Necropolis

2. Assessment of Condition

3. Materials and Methods

3.1. Materials

3.2. Samples Preparation:

3.3. Characterization of the Egg shell Nanoparticles

3.4. Preparation Method of the Egg shell Nanoparticles:

3.5. Application of Nano-Composite

3.6. Analyses and investigations

3.6.1. TEM investigation (Morphological study):

3.6..2 XRD analysis

3.6.3. FTIR spectroscopy:

4. Results and discussion

4.1. PLM Observation (BMM):

4.2. Observation and Analysis by SEM-EDX:

4.3. EDX Analysis:

5. Conservation Procedures

5.1. Pre-consolidation

5.2. Mechanical cleaning

5.3. Re-adhesion of detachment and cracks

5.4. Nano-Composite Result:

6. Conclusions

Declarations

References

Additional Declarations

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