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Influence of organosilicon compounds and

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stability of waterlogged elm wood

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Proceedings IRG Annual Meeting (ISSN 2000-8953)
© 2017 The International Research Group on Wood Protection

IRG/WP 17-10891

THE INTERNATIONAL RESEARCH GROUP ON WOOD PROTECTION

Section Y VVVVVVVVVV

Influence of organosilicon compounds and nanocellulose treatment

on dimensional stability of waterlogged elm wood

Magdalena Broda1, Bartłomiej Mazela1, Izabela Dąbek2, Agnieszka Dutkiewicz2,

Hieronim Maciejewski2, Roksana Markiewicz3, Mikołaj Grzeszkowiak3, Stefan Jurga3

Poznań University of Life Sciences

1

Institute of Wood Chemical Technology, Faculty of Wood Technology

38/42 Wojska Polskiego st., 60-637 Poznań, POLAND
2
Adam Mickiewicz University Foundation, Poznań Science and Technology Park
46 Rubież st., 61-612 Poznań, POLAND
3
Adam Mickiewicz University in Poznań, NanoBioMedical Centre
86 Umultowska st., 61-641 Poznań, Poland

Paper prepared for the IRG48 Scientific Conference on Wood Protection

Ghent, Belgium
4-8 June 2017

Disclaimer
The opinions expressed in this document are those of the author(s) and
are not necessarily the opinions or policy of the IRG Organization.

IRG SECRETARIAT
Box 5609
SE-114 86 Stockholm
Sweden
www.irg-wp.com
 Influence of organosilicon compounds and nanocellulose treatment on the
dimensional stability of waterlogged elm wood
Magdalena Broda1, Bartłomiej Mazela1, Izabela Dąbek2, Agnieszka Dutkiewicz2,
Hieronim Maciejewski2, Roksana Markiewicz3, Mikołaj Grzeszkowiak3, Stefan Jurga3
1
Poznań University of Life Sciences, Institute of Wood Chemical Technology, Faculty of Wood Technology, 38/42
Wojska Polskiego st., 60-637 Poznań, POLAND, mbroda@up.poznan.pl, bartsimp@up.poznan.pl
2
Adam Mickiewicz University Foundation, Poznań Science and Technology Park, 46 Rubież st., 61-612 Poznań,
POLAND, Izabela.Dabek@ppnt.poznan.pl, Agnieszka.Dutkiewicz@ppnt.poznan.pl,
Hieronim.Maciejewski@ppnt.poznan.pl
3
Adam Mickiewicz University in Poznań, NanoBioMedical Centre, 86 Umultowska st., 61-641 Poznań, POLAND,
roksana.markiewicz@amu.edu.pl, mikolaj.grzeszkowiak@amu.edu.pl, stjurga@amu.edu.pl

ABSTRACT

Commonly used agents for waterlogged wood consolidation (including the most popular
polyethylene glycol) have proved ineffective and even dangerous to the preserved objects,
jeopardising their integrity. Finding new, effective alternatives for safe preservation of wooden
cultural heritage is therefore of key importance. The future conservation agents should, first and
foremost, provide the integrity and dimensional stability of wooden artefacts and protect them
against biological degradation. They should also be chemically and mechanically stable and show
enhanced compatibility with wooden objects with no detectable side effects while being cheap,
renewable, and environmentally friendly.

Due to their unique attributes (e.g. excellent mechanical properties, biocompatibility, antifungal
properties, unique chemical reactivity, hydrophobicity), nanocellulose and some organosilicon
derivatives were used for the study to check their potential as consolidants for the conservation of
waterlogged wooden artefacts. Their influence on the dimensional stability of archaeological
waterlogged elm wood excavated from the bottom of the Lednica Lake in the Wielkopolska
Region was determined. The results clearly show that nanocellulose suspension applied alone is
not effective in wood stabilisation due to poor penetration of wood structure. In turn, some
organosilicons have a great potential for stabilisation of waterlogged wood dimensions. Four out
of eight tested derivatives demonstrated anti-shrink efficiency above 80%, while one of them
reached as much as 98.64%. This makes the organosilicon derivatives promising wood
consolidants, potentially useful in wood conservation practise. Therefore, further study on their
physical, chemical and mechanical properties will be undertaken.

Keywords: waterlogged wood, dimensional stability, organosilicon compounds, nanocellulose,

silanes
1. INTRODUCTION

In recent years, growing interest in developing new consolidants for conservation of wooden
archaeological artefacts has been observed. This is mainly due to the fact that in the light of current
scientific studies polyethylene glycol (PEG), the most popular conserving agent for waterlogged
wood, has proved ineffective and even dangerous to the preserved object. Despite its ability to
penetrate wood tissue and replace water molecules, thus reinforcing wood structure and improving
its dimensional stability, it also has a number of disadvantages (Hocker et al. 2012, Jensen and
Schnell 2005). First of all, it is easily leachable from wood under diverse temperature and humidity
conditions, which leads to irreversible deformations of wooden objects (Smith 2003). What is
more, PEG used as a conservation agent degrades to acidic by-products over time and can react
with other substances inside wood, causing chemical degradation, which contradicts its application
for wood conservation (Almkvist 2013, Almkvist and Persson 2007, Glastrup et al. 2006,
Sandström et al. 2005). High air relative humidity (over 80%) causes a sharp increase in PEG
hygroscopicity. As a result, wood impregnated with PEG absorbs water very intensively, which
leads to its strong swelling and cracking (Olek et al. 2016). Not without significance is also the
plasticising effect of PEG on already fragile archaeological wood (Bardet et al. 2007). Therefore,
finding a new, effective alternative to PEG for safe preservation of wooden cultural heritage is of
key importance. First of all, the future conservation agents should provide the integrity and
dimensional stability of wooden artefact and protect it against biological degradation. They should
also be chemically and mechanically stable and show enhanced compatibility with wooden objects
with no detectable side effects while also being cheap, renewable, and environmentally friendly.

Cellulose is the most common biomass in the world. It is composed of D-glucopyranose (C6H11O5)
units linked through β-(1,4) links, forming a disaccharide cellobiose – the repeating unit of
cellulose (Mariano et al. 2014). In nature, depending on the type of plant, cellulose concentration
reaches from 40% (in case of wood) to even 95% (in cotton). The unique structure of native
cellulose fibres held together by a lignin binder is responsible for the exceptional strength and
mechanical properties of plant cell walls. Cellulose nanomaterials can vary in shape and sizes,
forming nanowhiskers, nanofibrills, nanofibers, nanorods or nanocrystals. Characterised by unique
structural, mechanical and optical properties, they have already presented their potential in many
economy branches, including but not limited to packaging industry, water treatment technologies,
biomedical and energy areas, used also as food additives, personal care products and lightweight
composites (Carpenter et al. 2015). As a natural building block of wood, cellulose, and particularly
nanocellulose, seems to be a promising environmentally friendly material for conservation of
wooden artefacts. Due to its excellent mechanical properties (crystalline cellulose has greater axial
elastic modulus than Kevlar) and biocompatibility with wood it could be a great alternative for
commonly used reinforcement materials for wood conservation and restoration (Cipriani et al.
2010, Christensen et al. 2012, Moon et al. 2011, Walsh et al. 2016).

Due to their physiological neutrality, organosilicons are considered as environmentally friendly

compounds. Characterised by high thermal stability and chemical resistance to external factors
(humidity, UV radiation), they have applicability across many different branches of industry, e.g.
polymer, textile, building materials and pulp and paper industries (Brook 2000). Among the most
popular silicon derivatives are organofunctional silanes which are commonly applied as adhesion
promoters, binding agents and surface modifiers (Mittal 2009). The aforementioned compounds
are also used for conservation and protection of woodwork due to their unique chemical reactivity.
As a result of condensation with hydroxyl groups present on cellulosic fibres, the alkoxy groups
of organosilicons (that are susceptible to hydrolysis) enable to form stable siloxy bonds between
wood and a silicon compound (Donath et al. 2006, Donath et al. 2007, Hill et al. 2004, Mai and
Militz 2004, Mazela et al. 2013, Panov and Terziev 2009). Moreover, the presence of other

3
functional groups in the structure of the silicon compound makes it possible to modify the fibre
surface and impart specified functions to the cellulosic material. Organofunctional silanes are
commonly applied to modification of mineral surfaces, mainly silica. However, some differences
between hydroxyl groups present on the silica surface and those existing on surfaces of natural
fibres (including cellulose) should be kept in mind. In case of glass fibres (and other mineral fibres)
alkoxy groups undergo easy condensation due to acidic nature of Si-OH group (from glass fibres),
contrary to C-OH groups (from organic fibres). Furthermore, in the latter case condensation results
in the formation of alkoxy groups that can undergo a secondary hydrolysis. This is why the
modification of cellulosic material is conducted using also other silicon derivatives that contain
chemical groups capable of reacting with hydroxyl groups, e.g. isocyanate or epoxy ones, which
form considerably more stable bonds with cellulose (Przybylak et al. 2016). Beside
organofunctional silanes, modification of diverse materials can be performed using functionalised
polysiloxanes or silsesquioxanes. The former are characterised by durable, stable and, most
importantly, more flexible siloxane chain that enables a good orientation on the modified surface.
Moreover, various functional groups can be attached to the siloxane chain which allows formation
of a stable linkage with a substrate and, at the same time, imparts to its definite properties (Jones
et al. 2000). It is worth noting that silsesquioxanes are the latest generation of organosilicon
derivatives which, due to their strictly defined structure of nanometric dimensions and the presence
of diverse functional groups, permit surface modification and designing of desirable properties on
the molecular level (Hartmann-Thompson 2011). As the results of some research have shown that
organosilicon compounds can stabilise wood dimensions (Broda and Mazela 2017, Hill et al. 2004,
Smith and Hamilton 2001), all three types of the abovementioned organosilicon derivatives were
used for the study to check their potential as consolidants for the conservation of waterlogged
wooden artefacts.

The aim of the presented research was to determine influence of nanocellulose and organosilicon
compounds on the dimensional stability of waterlogged elm wood. Dating back to the 10th–11th
centuries, a waterlogged elm log was found at the archaeological site on the Ostrów Lednicki
island in the Wielkopolska Region (Broda et al. 2015). Excavated from the bottom of the Lednica
Lake, near the remains of the medieval “Poznań” bridge, the elm log was characterised by soft
structure and high degree of wood degradation, making it a perfect object for study on developing
new agents for waterlogged wood conservation.

2. MATERIALS

A waterlogged elm (Ulmus L.) log (Fig. 1) was cut lengthwise into quarters. Small square samples
(20 x 20 x 10 mm, radial x tangential x longitudinal direction) were cut out from the inner part of
the log (Fig. 2).

4
 Figure 1: Part of a waterlogged elm log excavated from the Lednica Lake

Figure 2: Wet elm wood samples

The reagents for nanocellulose and organosilicon derivatives synthesis were commercially
available and used without further purification. For synthesis and purification, the Milli-Q water
was used (conductivity below 0.055 µS/cm).

3. METHODS

3.1. Nanocellulose preparation

Cellulose rod-like nanoparticles were prepared according to the previously reported procedure
with several modifications (Ioelovich 2012). The sample of MCC was thoroughly mixed with
deionised water, and then 76% (w/w) sulfuric acid was carefully added to the mixture, so that the
required concentration of acid reached 60% (w/w). The acid to cellulose ratio was kept constant
and equal to 10. After that, the beaker with a mixture was put into an oil bath with constant
temperature (50oC) and stirring for 60 minutes. After that the reaction mixture was poured into
cold deionised water and stirred. Cellulose was separated from the mixture by centrifugation.
Cellulose nanoparticles were further washed with sodium bicarbonate solution (5–10%) and with
water to remove the sulfuric acid remains. Before each centrifugation, the cellulose particles were
disintegrated by ultrasound sonication.

3.2. Organosilicon synthesis

All organosilicon derivatives (labelled A–H) were obtained by hydrosilylation of relevant olefins
with Si–H-containing compounds (both hydrogen -silanes, -siloxanes or -silsesquioxanes) in the
5
presence of platinum catalysts, according to commonly known synthesis methodology (Marciniec
et al. 2009).

3.3. Sample impregnation

Wet elm wood samples were dehydrated with 96% ethanol for four weeks. Afterwards, they were
treated with one of the ethanol solutions: 1% nanocellulose suspension or 50% organosilicon
compound (A–H). Treatment by using the oscillated vacuum-pressure method consisted of 6
cycles: -0.1 MPa for 0.5 h and 1 MPa for 6 h/cycle. Untreated samples were used as a control.
After treatment all the samples were cured at ambient pressure and room temperature for 1 week.
Their pre- and post-treatment weight and dimensions in all three anatomical directions (tangential,
radial and longitudinal) were measured to calculate weight percent gain (WPG) and the anti-shrink
efficiency (ASE).

3.4. Scanning electron microscopy

Micro imaging of wood structure was performed using the Scanning Electron Microscope (SEM)
JEOL 7001F (Japan) with SEI detector at 1 kV or 5 kV accelerating voltage (depending of a wood
sample). Dry wood samples were precisely cut into smaller pieces and blown off with nitrogen to
remove the remaining dust. Afterwards, they were coated with a thin layer of chromium using high
vacuum coating system (240 secs), then mounted in the specimen holder and analysed.

3.5. Calculations
To assess effectiveness of the used treatment, the anti-shrink efficiency (as an indicator of
dimensional stability of wood) was calculated as follows:

S 0  S1
ASE   100 (1)
S0

where S0 is the volumetric shrinkage coefficient of the unmodified wood samples and S1 is the
volumetric shrinkage coefficient of the modified wood samples.

The percentage shrinkage coefficient of the unmodified wood (S0) was calculated as follows:

Vws1  Vd 1
S0  100 (2)
Vws1

where Vws1 is the water-saturated volume of the unmodified wood sample and Vd1 is the air-dry
volume of the unmodified wood sample.

The percentage shrinkage coefficient of the modified wood (S1) was calculated according to the
Equation 3:

Vwsm1  Vdm1
S1   100 (3)
Vwsm1

where Vwsm1 is the water-saturated volume of the modified wood sample and Vdm1 is the air-dry
volume of the modified wood sample.

6
ASE = 100% means that no wood deformation was observed. ASE values above 100% indicate
wood swelling, while those below 100% evidence shrinkage. In wood conservation practise, ASE
exceeding 75% is considered as acceptable (Grattan et al. 1980).

The weight percentage gain (WPG) of the wood samples was calculated according to:

W1  W0
WPG   100 (4)
W0

where W1 is the air-dry weight of the modified wood and W0 is the air-dry weight of the same
unmodified wood sample calculated on the basis of moisture content of wet unmodified control
samples.

4. RESULTS AND DISCUSSION

The results of waterlogged elm wood treatment as anti-shrink efficiency values are presented in
Figure 3. Out of the nine tested compounds, four reached ASE value above 75%, which makes
them potentially useful in wood conservation practise (Grattan et al. 1980). The remaining five,
including nanocellulose suspension, have not proved effective, reaching ASE value ranging from
39.91% to 70.76%. What deserves special attention is the great dimensional stabilisation of wood
(ASE˃80%) by four organosilicons: A, E, F and G. The best stabilising properties were observed
for organosilicon F. In this case ASE was 98.64%, which indicates almost unchanged dimensions
of waterlogged wood samples after treatment and air-drying and puts this substance on the top of
the list of the most promising wood consolidants unquestionably worth further study. For
comparison, the stabilisation effect of treatment with the most popular PEG usually ranges in ASE
values between 90% and 105%, depending on wood species, PEG type and the conservation
method applied (Babiński 2007, Babiński et al. 2017).

Figure 3: Anti-shrink efficiency of the treatment with the used compounds (NC – nanocellulose, A–H –
organosilicons)

7
Although the stabilisation effect of the chemicals used for waterlogged wood conservation is of
the greatest importance, the aesthetic attributes are not without significance. Post-treatment
coloration and samples appearance of air-dried waterlogged elm wood samples treated with
different test compounds are shown in Figure 4. In each case the least shrinkage occurred in the
longitudinal direction. The most prominent shrinkage, if it occurred, was observed in the tangential
direction. It resulted from the anatomical structure of wood: the specific structure of cellulose
microfibrils causes moisture changes mainly in the transverse direction (Kollmann and Cote 1968).
Tangential shrinkage was additionally impaired by the decay of the cellulose fraction (the loss of
wood substance in case of the waterlogged elm wood examined was about 70%), which made the
cell walls even more susceptible to collapse. The untreated wood samples (CU) shrank markedly,
one of the samples cracked in the middle, confirming the need to use the proper conserving agent
and method to preserve their shape and dimensions in an unaltered state. However, the samples
retained the natural colour of elm wood. In case of wood treated with nanocellulose suspension
(NC), irregular shrinkage was observed. The samples were coated with a thin layer of milky-white
nanocellulose lint, indicating poor penetration and deposition thereof on the surface of the sample.
Among samples treated with organosilicon compounds, the minor changes in shape and
dimensions were observed for A, F, E and G variants. No additional coatings were observed on
their surfaces; only A variant retained the natural elm wood colour, while F and G became lighter
and E dimmed slightly.

Figure 4: Dried waterlogged archaeological elm wood samples treated with nanocellulose (NC) and
organosilicon compounds: A, B, C, D, E, F, G and H, CU – untreated control sample

8
Figure 5: SEM images of dried elm wood samples treated with nanocellulose (N) and organosilicons (A–
H), CU – untreated control sample

9
SEM images in the cross-section of treated and untreated waterlogged elm wood (Fig. 5) revealed
differences in the internal structure of respective wood samples and in the way of deposition of the
conservation agents inside wood cells. The shape of untreated waterlogged wood cells was
irregular, with thin cell walls, indicating shrinkage (CU). The thickest cell walls, coated by some
additional layers of the used chemicals, and the most regular cell shape were observed for A, E, F
and G variants. It is consistent with the results of anti-shrink efficiency measurements and the
general appearance of these samples, confirming that dimensional stability results from the
structure. In case of B, C, D and H variants, some additional, more or less even coatings on the
cell walls were visible as well. Although, the shape of wooden cells remained irregular, indicating
the insufficient reinforcing properties of the used consolidants. In case of nanocellulose treatment,
thin cell walls and irregular shape of cells were observed, similar to untreated wood. Considered
in conjunction with the results of dimensional stability and the lint layer on the samples surface, it
confirms low penetration of nanocellulose into wood tissue.

5. CONCLUSIONS

The primary purpose in conservation of waterlogged archaeological wood is to preserve original

shape and dimensions of wooden artefacts. In light of this, seven out of the nine tested
organosilicon compounds fulfilled those expectations by reaching anti-shrink efficiency values
above 75%. Besides, most of them preserved the original appearance of elm wood in almost
unaltered state. This makes them potentially useful in wood conservation practise, although
additional studies are required to check their influence on other different properties of wood (e.g.
resistance to biodegradation and mechanical properties). If they meet all of the requirements, they
may become a promising alternative to polyethylene glycol or other currently used wood
consolidants.

Acknowledgement: The research was supported by the Polish Ministry of Science and Higher
Education as part of the “Cultural heritage – research into innovative solutions and methods for
historic wood conservation” project within the National Programme for the Development of
Humanities in 2015-2018 (project No. 2bH 15 0037 83).

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