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Consolidation of textile silk by spraying liquid silk proteins

Poster · July 2014

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Wojcieszak Marine Aline Percot

Royal Institute for Cultural Heritage Sorbonne Université
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Sylvie Noinville Philippe Colomban

French National Centre for Scientific Research Sorbonne Université
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 Consolidation of silk fabrics by fibroin spraying and
sericin dipping

Amandine Fraysse1, Marine Wojcieszak1, Aline Percot1, Sylvie Noinville1, Alba Marcellan2, Dominique de Reyer3,
Philippe Colomban1
1 "de la Molécule aux Nano-objets : Réactivité, Interactions et Spectroscopies" (MONARIS, ex-LADIR) - UMR 8233 - UPMC-CNRS Paris 06 - Paris
2 Laboratoire Matière Molle et Chimie - UMR 7167 – ESPCI Paris Tech-CNRS - Paris
3 Laboratoire de Recherche des Monuments Historiques (LRMH) - USR 3234 - Champs-sur-Marne
marine.wojcieszak@gmail.com

Introduction
Samples and methods
Many strategies have been developed to stabilize and consolidate historical material fabrics. Three methods are mainly used:
the traditional needle repair method, the adhesive consolidation and the use of wax/resins to reinforce the textile fibers.
Bombyx mori cocoons: for the preparation of silk solutions
Here, we propose new approaches by spraying liquid aqueous fibroin on fragile silk fabrics and dipping in sericin solution.
Silk fabrics: unbleached taffeta (40 threads/cm²)
Aim of the study: Aging conditions: Xenotest, 96h at 30°C and 60 % RH
► Solubilisation of silk proteins and characterization of the films obtained by evaporation on both sides (102 216 lux)
► Effect of silk coating solution on the mechanical properties of silk fibers Characterization: Raman spectroscopy - tensile testing
► Consolidation of artificially aged silk fabrics by spraying/dipping liquid silk proteins

Silk composition Films, composites & consolidation

Silk = protein fibers  wide range of fibers created by different types of organisms Characterization and properties of fibroin films
degummed fiber
not filtered (D) Amide I band 100 degummed fiber
Fibroin: filtered (O) ~ v C=O

Raman intensity
not filtered (D)
Silkworm bave 80 filtered (O)
Bombyx Mori Natural polyamide

Stress / MPa
~ 20 µm
(domestic) Length > 1000 m 60
O H O R H
C CH2 N CH N 40
N CH N
Sericin 2 fibroin H O CH3 H O 20
coating fibers Gly Ala Amide Bond
LabRam HR 800, 514 nm 0
1500 1600 1700 0.0 0.5 1.0 1.5
" Repeating units " Wavenumber / cm
-1
Strain / %
Yarns & textiles Gluing and Mechanical (GAGAS)5-15(GX) 5-15GAAS* Consolidation of artificially aged fabrics Effect of fibroin solution on silk fibers
protection properties
Spraying method: Dipping method:
(hydrophilic) (hydrophobic)
Fibroin solution
(filtered)
Preparation of silk solutions and films** Silk solutions
+
10 mm

Silk fibre
reinforced silk
Na2CO3 0,023 mol/L 4.5 mL of filtered Sericin solution Directionally matrix composite
~ 95°C fibroin solution ~ 10 g/L ~ 2 g/L oriented fibers

0. Degumming 1. Solubilisation + + 1 mm

30 mm
Sericin LiBr 500 degummed fiber
5 mm fibers extracted from composite
9 mol/L
Cocoons 2+4 Fibroin fibers 2 or 3 sprays applied Dipping for 400
45°C 5 times on each side 1 hour at RT
Stress / MPa

2. Dialysis Porosity Dried at RT

300

Regenerated silk films 0,5 µm 25-30 Å

200
- Sericin films 3. Filtration + 4 LiBr
O
-Two types of fibroin films 100

(Ordered and Disordered) Room temperature (RT)

and humidity Fibroin solution 0
D Artificially aged fabric Artificially aged fabric 0 5 10 15 20 25
4. Evaporation Concentration with fibroin coating with sericin coating Strain / %
~ 15 g/L
1 mm Stress-strain curves of fabrics Summary table

Young’s Strain to
Preparation of artificially aged fabrics 50 Sample modulus
Strength
failure
reference / MPa
Instrument: ST-10 Monsanto, cross head speed: 2 mm/min artificially aged / GPa /%
artificially aged + fibroin
reference
40
artificially aged + sericin
degummed fiber *** 5-10 320-1410 4-35
 fibers are well organized
Stress / MPa

40 artificially aged fibroin film

and it is easy to distinguish 30 4 43 1.2
(filtered, O)
warp and weft
Stress / MPa

30 fibroin film
20 1.2 9.2 0.8
reference (not filtered, D)
20 reference frabric ND 32-39 24-26
10
 variability and loss of aged fabric ND 8-31 10-20
10 0
mechanical properties aged fabric +
0 10 20 30 40 ND 13-17 16-18
fibroin (7-8 % w/w)
0 Strain / %
artificially aged aged fabric +
0 10 20 30 40 ND 30-37 25-27
Strain / % sericin (0.5-2 % w/w)

Conclusions References:
* Inoue, S., Tanaka, K., Arisaka, F., Kimura, S., Ohtomo, K. and Mizuno, S. (2000). "Silk
Fibroin of Bombyx mori Is Secreted, Assembling a High Molecular Mass Elementary Unit
 Optimization of fibroin solution: fibroin films from filtered solutions are less organized but show improved mechanical Consisting of H-chain, L-chain, and P25, with a 6:6:1 Molar Ratio." Journal of Biological
Chemistry 275(51), 40517-40528.
properties. ** Colomban, Ph., Moukit, S.E., Dinh, H. M., Hassine, M., Riand, J., and Mauchamp, B.
(2008). "Micro- & Nanomécanique des fibres naturelles (animales)." Revue des
Composites & Matériaux Avancés 18(2), 163-168.
 Effect of fibroin matrix on silk fibers: the mechanical properties of fibers extracted from the composites are not altered. *** Colomban, Ph., Dinh, H. M., Bunsell, A. and Mauchamp, B. (2012a). "Origin of the
variability of the mechanical properties of silk fibres: 1 - The relationship between
 Weak improvment of strain to failure for artifically aged fabrics reinforced with fibroin but decrease of variability. disorder, hydration and stress/strain behaviour." Journal of Raman Spectroscopy 43(3),
425-432.
Pérez-Rigueiro, J., Viney, C., Llorca, J. and Elices, M. (2000). "Mechanical properties
 With sericin, artificially aged fabrics recover their initial properties ; the important role of sericin was already observed for of single-brin silkworm silk." Journal of Applied Polymer Science 75(10), 1270-1277.
**** Jauzein, V. and Bunsell A. (2012) "Bio-composite aspect of silk: the sericin sheath
industrial yarns****. acting as a matrix." Journal of Materials Sciences 47(7), 3082-3088.

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