10

Surface Modification of Wood

10.1 Introduction
Due to increasing concerns on global warming, the forestry policies have
been laid down globally to conserve forests and to halt the loss and deg-
radation of forest ecosystems. In order to achieve this goal to promote
and restore forests, environmentally sound forest harvesting practices are
adopted. This is reflected in the restricted availability high quality of wood
raw materials to the wood industry. As a result, wood of large diameters
are no longer easily available for the production of veneer-based compos-
ites. The industry is therefore compelled to use secondary species of poor
quality with gums or resins on the surface, which have adverse effect on
bonding. In addition, drying veneers at high temperature to increase pro-
duction and save energy results in the inactivation of veneer surfaces due
to reasons discussed in Chapter 8. In order to obtain a better performance
with the available raw materials, the surface modification of veneers is
necessary [1].
Surface modification of wood is defined as the application of a chemi-
cal, physical, or biological agents to the wood surface in order to obtain a
desired improvement of performance [2, 3]. The improvement of perfor-
mance may be effected by modification of the surface energy in order to
improve adhesion. Wood surfaces can be treated by plasmas from various
sources, by chemical or enzymatic grafting of functional groups or by coat-
ing by either sol–gel methods, or deposition of nanoparticles. The target
properties to be improved are surface activation for better wettability, glu-
ing and adhesion of surface coatings, and resistance to weathering.
Surface modifications are important not only for solid wood and veneers
but also for wooden particles, wood-based fibers, and other non-wood lig-
nocellulosic fibers. They are mainly intended to improve adhesion between
the lignocellulosic particles/fibers and thermoplastic matrices in wood–
polymer composites.

R. N. Kumar and A Pizzi. Adhesives for Wood and Lignocellulosic Materials, (223–238) ©  2019
Scrivener Publishing LLC

223
224 Adhesives for Wood and Lignocellulosic Materials

10.2 Surface Modification Methods

10.2.1 Plasma and Corona Treatments
One of the technologies to improve the surface characteristics of wood is
the plasma treatment [4]. The purpose of plasma treatment is to improve
adhesion. The plasma technology has recently attracted research interest
in many countries [5, 6]. It has also been applied to lignocellulosic fiber
panels [7].
Plasma can be described as partially ionized gas consisting of a complex
mixture of ions, electrons, ultraviolet photons, and reactive neutrals such
as radicals, excited and ground state molecules, etc. [8]. In other words,
plasma is a collection of all the abovementioned species. Plasma is usually
generated from gases by the absorption of enough energy to cause the elec-
trons to become separated from their nuclei, resulting in ionization and
fragmentation. When this happens, the plasma no longer acts like a gas.
Plasma, as characterised by particles with very low degrees of ioniza-
tion and little penetrating energy (called cold plasma), is often used for
surface modification or activation [18]. Excited particles in cold plasma
have energy levels (0.5–3 eV) sufficient to break chemical bonds on the
surface of organic and inorganic substrates [9, 10]. These broken chemical
bonds are thermodynamically unstable and combine with ambient mole-
cules to re-engineer the surface of the material [11]. This type of modifica-
tion (cleaning, etching, or cross-linking), however, is limited to the surface,
typically to a depth of a few molecular layers. Plasma is also considered to
be the fourth state of matter because it is more highly activated than solid,
liquid, or gaseous states.
More detailed definitions of plasma have appeared in the literature
[12–14].
The characteristic behavior of plasma depends on the ratio of ionized to
neutral particles and the particle energies. These characteristics lead to a
broad spectrum of plasma types.
Plasmas can be classified either as:

(1) Equilibrium plasmas (also called thermal or hot plasmas,

with high degrees of ionization) or
(2) Non-equilibrium plasmas (also named non-thermal or
cold plasmas, with low degree of ionization).

In equilibrium plasmas, the temperature of electrons and of the gas is

the same, and can be as high as 10,000°C. In non-equilibrium plasmas, the
 Surface Modification of Wood 225

gas is at ambient temperature, but the temperature of electrons is very high,

of about 10,000°C [6, 7, 12, 15].
Thus, a plasma is referred to as being “hot” if it is nearly fully ionized,
or “cold” if only a small fraction (for instance 1%) of the gas molecules are
ionized, but other definitions of the terms “hot plasma” and “cold plasma”
are common. As mentioned above, even in cold plasma, the electron tem-
perature is still typically several thousand degrees centigrade [16].
Plasmas transfer energy to the surfaces, thereby effecting surface modi-
fication. In order to sustain the plasma state, energy must be continuously
injected into the system. The easiest way to ensure this requirement is by
using electrical energy [12, 17]. An electrical field is necessary to generate
a plasma. In a vacuum chamber, the ions and electrons have long lifetimes.
Radio-frequency power can be applied to two metal plates immersed in the
vessel, creating a capacitive discharge.
Gas discharge plasmas, also known as low-temperature plasmas, have
drawn much attention in the past few decades because of their importance
in many technological developments. A dielectric barrier discharge (DBD)
plasma generator functions due to electrical discharge between two elec-
trodes separated by an insulating dielectric barrier. It was originally called
silent discharge and is also known as ozone production discharge.
Because of the unique characteristics of plasmas, a growing number of
applications have emerged [18]. The species in plasma that modify materi-
als are electrons, ions, and radicals. The latter two species are generated by
collisions between electrons and gas molecules existing in plasma.
Two categories of plasma, the thermal and non-thermal ones, can be
defined according to the conditions in which they are created.
Thermal plasmas are obtained at high pressure (≥105 Pa) and need sub-
stantial power (up to 50 MW). Non-thermal plasmas are obtained at lower
pressures and use less power. Such plasma can be generated by electric
discharges in gases at low pressure.
Over recent years, atmospheric plasmas have been developed that are
now available for industry use. This technique is already used in the plas-
tic and glass industries to improve adhesion between coating and sub-
strate by modifying substrate surface energy or/and grafting new chemical
functions.
Plasma treatment technology is simple and has low operating costs. In
addition, there is no environmental pollution created by this treatment
process, and it has a very promising future for engineering applications.
Plasma treatment only affects the near surface of a material without chang-
ing bulk material properties, as opposed to chemical modifications [19,
20]. The plasma treatment system is described by Aydin [4] and Petric [2].
226 Adhesives for Wood and Lignocellulosic Materials

The application of plasma in wood and wood-based materials has two

main goals: (1) the improvement of adhesion [21–25] and (2) the depo-
sition of low-surface-energy thin films to increase the barrier properties
against polar and nonpolar liquids and gases. It is a dry and a clean process
with little environmental impact.
Plasma modification causes increased surface polarity induced by oxi-
dation reaction, leading to the formation of hydroxyl, carboxyl, aldehyde,
and other polar functional groups [26].
Improvement of specific surface properties in the case of plasma treat-
ment depends on the plasma reactor’s design, the plasma gases used, and
plasma treatment parameters. Examples of such properties are wood wet-
tability, water repellence, surface free energy, the adhesion strength, and
biocompatibility [14] and coating adhesion. Plasma can also alter the sur-
face properties even of normally inert materials such as ceramics [13]. The
plasma gas is probably one of the most important parameters. Inorganic
plasma gases such as nitrogen, oxygen, carbon dioxide, air, water vapor,
argon, and others are generally used to alter surface properties such as
wettability.
Over recent years, atmospheric plasmas have been developed that are
now available for industry use. This technique is already used in the plas-
tic and glass industries to improve adhesion between coating and sub-
strate by modifying substrate surface energy or/and grafting new chemical
functions.
It is well known that a wood surface exposed to contaminants such as
dust or atmospheric grime can experience surface inactivation that can
reduce the attractive forces on the wood surface and lead to a decrease in
wettability. But it was shown that low-pressure O2 plasma treatment can
reactivate the surfaces of spruce wood for adhesive bonding and to increase
wettability even after a 9-year period of natural surface inactivation. Thus,
the target properties to be improved or even introduced are mostly surface
activation for better gluing and adhesion of surface coatings, wettability,
and resistance to weathering.
Different gas species can be used in plasmas in order to obtain the
desired surface properties, by influencing the interactions between the
gas and the solid surface depending on the nature of the gas species used
in plasma. Some gas species can change the surfaces into hydrophobic,
whereas other ones create hydrophilic surfaces [27]. One of the most pop-
ular gas species used in plasma influencing wood surfaces is oxygen, with
a target to improve adhesion [4, 28]. Oxygen plasma has also been used
for cleaning different areas such as micro-electro-mechanical systems.
Literature contains some studies about the effects of plasma treatment with
 Surface Modification of Wood 227

different gas species on adhesion properties [29], contact angle [4], wetta-
bility, and bonding.

10.2.2 Corona Treatment

The non-equilibrium plasmas are classified roughly into two categories:
(a) ordinary low-temperature plasmas generated at low pressure, also called
“glow discharge”, and (b) corona discharges at atmospheric pressure [12].
Glow discharges are the most widely used technique for low-temperature
plasmas. The reason is that the mean free path of activated gas molecules
is longer in vacuum, which allows the use of a bigger distance between the
electrodes and the samples. This kind of plasma has been used as a highly
effective pretreatment for the surface preparation of low-surface-energy
polymers for adhesive bonding [6].
The corona discharge treatment (CDT) has a more restricted appli-
cation range, since it is limited to the materials that are responsive to
this method of surface treatment and the material configuration (geom-
etry). Complex shapes cannot easily be treated because the treatment
quality is a function of the distance of the surface to the electrode. Also,
since corona treatments are normally conducted in ambient air, they
can be affected by environmental changes in the location where it takes
place. The main advantages of CDTs are that, since no vacuum system is
needed, the equipment investment is much lower than that for ordinary
low-temperature plasma installations. In CDT, the discharge is generated
by applying a high-frequency, high-voltage signal to an electrode that is
separated from an earthed plane, usually by only a few millimeters, by an
air gap, the substrate, and a layer of dielectric material [6].
Uehara and Jodai [30] found that the joint strength of corona-treated api-
tong (Dipterocarpus grandiflorus Blanco) bonded with urea–formaldehyde
adhesive increased with the corona treatment. However, the results for the
phenol–resorcinol–formaldehyde (PRF) resin were different. After the treat-
ment, the wettability by the PRF resin did not improve and no improvement
in the joint strength was observed.
Back studied the effects of the corona discharge on the wettability of
teak, birch, and pine (Pinus sylvestris L.) [31]. The treatment resulted in
a significant increase in the wettability of teak and birch, but the effect
on pine was minimal. It was concluded that the CDT could be used to
improve the wettability of timbers with high resin or oil content and also
to treat wood surfaces that have undergone thermal aging.
Sakata et al. (1993) have shown that the treatment by corona of the
surface of several softwood, hardwood, and tropical wood veneers caused
228 Adhesives for Wood and Lignocellulosic Materials

a considerable increase in the wettability of the surface by the urea resin

and the improvement in the adhesion of veneers with water-based adhe-
sives [32]. An increase in the wettability of corona-treated wood veneers of
hardwoods, softwoods, and tropical woods was observed. The wettability
increased with an increase in the degree of treatment. This is attributed
to the oxidation of the highly hydrophobic surface layer. To elucidate the
nature of any chemical change occurring on the wood surface, the dyeing
examination of the wood and its components with Schiff ’s reagent was car-
ried out, and the results showed a high degree of dyeing ability for corona-
treated samples as compared to untreated ones, thereby indicating that
aldehyde groups increased as a result of the corona treatment.
Thus, the wettability of corona-treated wood veneers resulted mainly
from the oxidation of the high hydrophobic surface layer.

10.2.3 Plasma Applications for Wood Surface Plasma Treatments

Some applications have been investigated. Podgorski et al. studied the
influence of various plasma treatments on several fir species [33]. They
showed that adhesion of coatings could be improved. Rehn et al. showed
that the fracture strength of glued black locust (Robinia pseudoacacia)
could be increased and coating delamination reduced [34]. The fire and
moisture resistance of different Philippine species were improved after
hydrogen plasma treatment by Blantocas and Al-Aboodi [35]. Evans et al.
investigated the impact of plasma treatment on the wettability and glue
bond strength of four eucalyptus species [36]. Finally, Wolkenhauer and
coworkers studied several properties of wood after plasma treatments [29,
37]. In 2009, they demonstrated that a plasma treatment of wood surfaces
was superior to sanding for increasing surface energy [29].
Wolkenhauer et al. [29, 37] carried out the surface treatment of beech,
oak, spruce, and Oregon pine wood by plasma produced by DBD and com-
pared the surface characteristics of the plasma-treated wood with those
of sanded surface. The surface energy of aged, freshly sanded, or plasma-
treated surfaces was examined by contact angle measurement and calcu-
lation of work of adhesion. Plasma treatment turned out to be superior to
sanding.
The increase in surface energy was caused by an increased polar group
on the surface. To see whether a combined treatment amplified this effect,
a combination of sanding and plasma treatment was also investigated.
Avramidis et al. [38] carried out the plasma treatment at atmospheric
pressure using a DBD in order to increase the surface hydrophilicity of
wood and wood-based materials. Surface energy determination by contact
 Surface Modification of Wood 229

angle measurement revealed an increase in the polar component of sur-

face energy and in total surface energy following plasma treatment. X-ray
photoelectron spectroscopy revealed an increase in O/C ratio, indicating
the generation of polar groups. An atmospheric-pressure plasma jet using
hexamethyldisiloxane as precursor and air as process gas was used for
thin-layer deposition.
The feasibility of plasma polymerization on wooden substrates at
atmospheric pressure to create water-repellent characteristics was also
investigated. Atomic force microscopy revealed a closed surface layer con-
sisting of silicon, oxygen, carbon, and hydrogen that exhibited low water
permeability.
Aydin et al. [4] enhanced the ability of the inactivated wood surfaces
for better adhesion and bonding by employing plasma treatment. In their
studies, a low-pressure plasma treatment was applied to reactivate the sur-
faces of spruce wood for glue bonding and to increase wettability after a
9-year period of natural surface inactivation. The inactivation was found
to have been caused by contaminants such as dust or atmospheric grime
due to the exposure of the surface to atmosphere over a long period of
time. The inactivation mechanisms were proposed to be due to reduction
of the attractive forces on the wood surface that leads to a decrease in
wettability. Changes in contact angles, surface energy, surface color, and
bonding strength of inactivated and oxygen plasma-treated wood surfaces
were studied. Wettability, bonding, and other mechanical properties of
plywood panels produced from the wood veneers treated with the oxy-
gen plasma were increased .Thus, plasma treatment has been applied to
recover inactivated wood surfaces for better adhesion and bonding. As
mentioned earlier, the plasma treatment technology is very simple and the
cost is rather low. In addition, this treatment produces no environmental
pollution.
In their study on the surface treatment of Pinus yunnanensis wood,
Fang et al. used microwave plasma [39].The microwave plasma presented
very significant treatment effects on the treated surface, even under weak
treatment conditions. The treated surface showed better surface wettabil-
ity. The contact angles on the treated surface measured from deionized
water, glycerin, and diiodomethane decreased sharply, even to 0°. The
treated surface also presented higher surface free energy, for example,
61.4–62.8 mJ m−2, being greatly improved by microwave plasma compared
to that of untreated surface of 46.5 mJ m−2. The bond strength of the treated
surface was 7.34 MPa, about 16% higher than 6.31 MPa for the untreated
surface. The authors recommend that this technique might be widely used
in wood modification and wood processing.
230 Adhesives for Wood and Lignocellulosic Materials

Acda et al. reported on the effects of plasma modification on surface

properties of three species of wood [26, 28]. The authors made use of DBD
to modify the surface properties of Shorea contorta, Gmelina arborea, and
Acacia mangium commonly used in the Philippines and Southeast Asia for
furniture and wood-based panel manufacture. Wood specimens exposed
to oxygen plasma resulted in a several-fold increase in surface free energy.
They also reported that cold plasma treatment induces physical and chemi-
cal changes to the depth of a few micrometers on the wood surface without
any change in bulk properties [14]. Cold oxygen plasma, which is com-
monly used to improve wood surface, can react with wood to produce a
variety of oxygen functional chemical species such as C–O, C=O, O–C=O,
C–O–O, and CO3 at the surface [40].
No apparent surface defects or changes in bulk properties were
detected. The increased surface free energy could be positively correlated
with the development of good joint strength during gluing with polar
adhesives.
Cold plasma has been found to be a powerful tool that can be used to
improve the wetting and adhesion properties of wood [26, 28, 36, 41, 42]
and wood composites [37, 43, 44]. It is believed that plasma modification
results in increased surface polarity brought about by the formation of
hydroxyl, carboxyl, aldehyde, and other polar functional groups [45]. The
increased surface polarity improves wettability and penetration behavior
(hydrophilicity) of wood to liquid [34]. The wettability assists in establish-
ing extensive and molecular-scale contact with the wood surface, which is
critical to the development of strong adhesion at the adhesive–wood inter-
face and also for the coating adhesion [33, 34, 36, 41, 42, 46–48].
Wascher et al. reported that the five-layer plywood boards made from
plasma pretreated veneers exhibited up to 2.7-fold improvement in shear
strength compared to plywood made of untreated veneers [49].
Wolkenhauer et al. investigated the adhesion of PVA glue on fiberboard
and particle board in the untreated state and plasma-treated with a DBD
at atmospheric pressure [37]. A force-sensitive peel test was carried out
and confirmed increased adhesion after plasma treatment.

10.3 Enzymatic Modification for Hydrophobicity

Preparation of wood thermoplastic polymer matrix composites requires
hydrophobization of the lignocellulosic fibers by suitable surface
modification so as to impart compatibility with thermoplastic poly-
mers. Chemical modifications and plasma treatment of the fibers are
 Surface Modification of Wood 231

currently adopted. Enzymatic modification can be an attractive alterna-

tive for increasing lignocellulose hydrophobicity. An example is laccase-
mediated grafting of laurylgallate onto pulp, which has increased its
hydrophobicity [50].
Laccase-catalyzed coupling of fluorophenols was shown to increase
hydrophobicity of wood veneers [51]. The authors also provided the
first in vitro evidence for the possibility of establishing covalent bonds
between complex lignin model compounds and the fluorophenols, which
were found to bond to sinapyl units via 4–0–5 linkages while coupling
to guaicyl units occurred through 5–5 linkages. The same authors also
elegantly demonstrated the ability of laccase to couple long-chain alkyl-
amines onto wood veneers, resulting in an increase in hydrophobicity
[52]. Research has been focused on the application of laccases toward
functionalization of pulps in order to produce novel paper products. The
pioneering works of Yamaguchi and coauthors [53–55] demonstrated
the ability of laccase to polymerize various phenolic compounds to form
dehydrogenative polymers, which were subsequently coupled to thermo-
mechanical pulps in the presence of peroxidase. Incorporation of phe-
nolics (vanillic acid, catechol, mimosa tannin, and tannic acid) in the
presence of laccase enabled production of paper with increased tensile
strength and water-resistant properties attributed to the coupling of free
phenolic groups on the fiber surface with the added dehydrogenative
polymers. The progress made in the field of laccase-assisted biograft-
ing has been outlined above in order to show the potential for further
exploitation of laccases to the future development of environmentally
friendly adhesively bonded materials.

10.4 Modification of Wood Surface by Chemical

Treatment—Functionalization of Wood
The term grafting is considered to represent covalent bonding of various
substances, very often polymers or monomers.
In the case of wood, these are predominantly cellulose and lignin.
Roman-Aguirre et al. and Wang and Piao define grafting as a molecular
technique that chemically bonds foreign molecules to a surface [56, 57].
An example is to use a silane coupling agent. The coupling agents contain
alkoxy groups that react with wood hydroxyl groups by initially converting
the polar OH groups of wood via Si–O–C (wood) linkages into the hydro-
phobic moiety. An analogous approach with alkoxy-terminated silicones
has been described for the hydrophobization of proteins [58–61].
232 Adhesives for Wood and Lignocellulosic Materials

The disadvantage of the use of such silane coupling agents is that

Si–O–C linkages are formed between wood and the hydrophobic moi-
ety. However, Si–O–C bonds are normally subject to hydrolysis, giving
silsesquioxanes (R-SiO3/2), limiting the degree of hydrophobization [62].
Sebe and Brook have adopted a method in which grafting relies on the
formation of covalent bond, viz., Si–C–O–C (wood), linkages that are
not so susceptible to hydrolysis [63].
In this method, the wood is initially treated with maleic anhydride or
allyl glycidyl ether. This reaction resulted in oligoesterified wood bear-
ing terminal alkenes (see the reaction scheme, Figure 10.1). The terminal
alkenes are reacted with hydride terminated silicones. Hydrosilylation
reaction leads to a wood–silicone moiety containing Si–C–O–C (wood)

O
OH CH2 O CH2 CH=CH2
Wood + H2C CH
Allylglycidylether

OH

O CH2 CH CH2 O CH2 CH=CH2

Wood

H-Si Hydrosilylation

OH

O CH2 CH CH2 O CH2 CH=CH2

Wood

H-Si Hydrosilylation

OH

O CH2 CH CH2 O CH2 CH2 CH2 Si

Wood

Reaction scheme for hydrophobization of wood

Figure 10.1 Hydrophobization of wood.

 Surface Modification of Wood 233

linkages, which are hydrolytically more stable than the Si–O–C linkages
formed by using the conventional silane coupling agents. Hydrosilylation
results in the formation of hydrophobic surfaces that remained unim-
paired even after extensive soxhlet extraction with good solvents for
silicones.
In order to convert the hydrophilic surface of bamboo flour into a
hydrophobic surface, Yu et al. employed atom transfer radical polymer-
ization method by which methyl methacrylate was grafted onto the bam-
boo flour surface [64].

10.5 Sol–Gel Method

Another method for the surface modification of wood is to conduct the
chemical reaction of the reagent Si(OEt)4 or Cl-Si(OEt)3, which is more
reactive than Si(OEt)4 with lignocellulosic substrate by base/acid-catalyzed
hydrolysis to form a wood-bound silica composite with glass-like surface
properties. This method is a better alternative to reacting the lignocelulosic
substrates with silane coupling agents. As mentioned in Section 10.4, silane
coupling agents form C–O–Si linkages.
Although application of silane coupling reagents for improvement of
wood flour and wood-derived fiber polymer composites dates from 1983,
the hydrolytic stability of the C–O–Si has not been considered seriously.
The silane coupling mechanism per se depends on the hydrolytic suscepti-
bility of the Si–O–C bonds in Si–OC2H5, which readily hydrolyzes to form
the -Si–OH groups in the presence of acids or alkalis. The result is the for-
mation of a C–O–Si covalent bond formed between cellulose and silicon
that is not hydrolytically stable.
A new sol–gel strategy can be applied to enhance adhesion between
wood/lignocellulosic fibers and polymeric adhesives or matrix mate-
rials. By this new process, glass-like surface properties can be first
imparted onto the wood or lignocellulosic fibers followed by the addi-
tion of silane coupling reagents, which will result in the formation of a
Si–O–Si–C bond between wood and the organic polymeric adhesives or
matrix materials.
The traditional sol–gel process involves the chemistry of metal alkox-
ide precursors, such as silicon alkoxides, and similar metal alkoxides, such
as titanium, aluminum, and zirconium, resulting in amorphous inorganic
materials [2, 65].
The sol–gel reactions are given in the Scheme in Figure 10.2.
234 Adhesives for Wood and Lignocellulosic Materials

1. Formation of reactive species

OC2H5 OC2H5

C2H5-O Si OC2H5 + H2O C2H5-O Si OH

OC2H5 OC2H5

2. Sol formation-Polycondensation
OC2H5 OC2H5 OC2H5
OC2H5
C2H5-O Si O* Si O Si OH
nC2H5-O Si OH
H2O
OC2H5 OC2H5 OC2H5
OC2H5
n-1
Sol

3. Gel formation

OC2H5 OC2H5 OC2H5

C2H5-O Si O* Si O Si OH

OC2H5 OC2H5 OC2H5

n-1
Sol

O O O

O Si O* Si O Si O

O O O
n-1

Gel

Figure 10.2 Sol–gel reaction scheme.

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