Vacuum 146 (2017) 649e654

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Vacuum
journal homepage: www.elsevier.com/locate/vacuum

Fabrication and characterization of transparent wood for next

generation smart building applications
Haritha Sree Yaddanapudi, Nathan Hickerson, Shrikant Saini, Ashutosh Tiwari*
Nanostructured Materials Research Laboratory, Department of Materials Science and Engineering, University of Utah, Salt Lake City, Utah, 84112, USA

a r t i c l e i n f o a b s t r a c t

Article history: A major fraction of the electricity that is generated in the world is used in the building sector, particularly
Received 19 October 2016 as a source of light. One way to reduce the consumption of electricity in buildings is by utilizing natural
Received in revised form light with the help of environmentally friendly resources such as transparent wood. Removing the lignin
4 January 2017
from wood followed by impregnating environmentally friendly polymers whose refractive index
Accepted 7 January 2017
matches the refractive index of the cell wall helps in obtaining transparent wood. Hence, herewith we
Available online 19 January 2017
report a simple and low-cost method of fabricating transparent wood from beech wood (Fagus gran-
difolia) while retaining its 3-dimensional structure. The surface morphology of the synthesized trans-
Keywords:
Transparent wood
parent wood was studied by using scanning electron microscopy. Brunauer Emmet Teller measurements
Energy consumption were carried out to determine the specific surface area. FTIR measurements were performed to study the
Environment-friendly wood chemistry. Optical measurements showed a maximum optical transmittance of 70% and a
Energy management maximum haze of 49% for 0.1 mm and 0.7 mm thick wood samples, respectively. Mechanical testing
showed that the transparent wood has a higher tensile strength and hardness when compared to the
delignified wood. The fabricated transparent wood with high transmittance and enhanced mechanical
properties is a potential candidate material for light transmitting building materials and transparent
solar cell windows.
© 2017 Published by Elsevier Ltd.

1. Introduction growth process, possesses excellent mechanical properties relative

Due to the enlargement of the global economy, there is an in-
crease in the demand for energy consumption. A majority of this
energy is supplied through fossil fuels such as coal, oil, and natural
gas which result in the production of green-house gases and con-
tributes to global warming. According to recent reports, the global
temperature has been increasing continuously over the past 100
years [1,2]. According to the US department of energy resources, the
U.S consumes about 47.6% of its energy through the building sector,
24.4% through industry and 28.1% through transportation [3e5].
One way to reduce the amount of energy being consumed through
the building sector is to design semi-transparent buildings. These
buildings can potentially reduce the utilization of artificial light by
substituting it with the natural light. Furthermore, since they are
not completely transparent, privacy is still retained.
One of the materials that plays a major role in the building
sector is wood. Wood, due to its unique structure and natural
* Corresponding author.
E-mail address: tiwari@eng.utah.edu (A. Tiwari).
to its cost. These include a high strength, good durability, high
moisture content, and high specific gravity. Based on its structure,
availability, and geographical differences, wood is classified into
two types. They are the soft wood and hard wood. Soft wood has a
high porosity due to its faster growth. Soft wood mainly includes
cedar, pine, spruce, and redwood. In contrast to soft wood, hard
wood has a higher density and is denser in structure [6]. Moreover,
the longitudinal cells are shorter in length when compared to those
in hard wood. However, both soft and hard woods possess similar
hierarchical structure. In other words, the orientation of the cells is
similar in the wood [7].
The structural anisotropy is a unique property of a wood. This is
due to the alignment of the vertical channels across the cells pre-
sent in the wood. It allows to pump ions and water for photosyn-
thesis. Cells in the wood are mainly composed of cellulose which is
a long chain of polysaccharides molecules containing at least 40% -
50 % glucose. Cellulose is also made up of lower molecular weight
polysaccharide chains called hemicellulose. Lignin is the other
major component that is present in the wood. It accounts for about
25% of the wood structure. It mainly acts as a glue which helps in

http://dx.doi.org/10.1016/j.vacuum.2017.01.016
0042-207X/© 2017 Published by Elsevier Ltd.
650 H.S. Yaddanapudi et al. / Vacuum 146 (2017) 649e654
bonding all the wood cells together. Furthermore, lignin provides
high hardness and rigidity to the wood. Cellulose, which is the
major component in wood, plays a vital role in development of
flexible electronics such as optoelectronic devices. However, to
make an optoelectronic device, the wood should be transparent to
the relevant spectrum.
As mentioned earlier, the main components of wood are cellu-
lose, hemicellulose and lignin. In contrast to cellulose and hemi-
cellulose which are colorless, lignin possesses an extremely dark
color. Therefore, this dark color leads to light scattering over the
visible range. One way to make the wood transparent is to bleach it,
which helps in removing the lignin and pulp. However, since all the
color across the pores in the wood are not removed, polymer which
can provide strength and transparency is impregnated into the
pores of the wood which run vertically down. Several recent
attempt have successfully been made to fabricate transparent
wood. However, the process to fabricate transparent wood ob-
tained so far is complicated and requires environmentally un-
friendly reagents [8e12].
In this study, our objective is to develop a transparent wood
from beech wood (Fagus grandifolia) using a novel two-step syn-
thesis process. In a recent study, the wood-PMMA composite ma-
terial [13] was shown to exhibit a high durability with excellent
mechanical properties. In this paper, we report the synthesis of
optically semi-transparent wood which possesses an optical
transmittance of 60% along with a haze of 49%. Furthermore, its
mechanical and microstructural properties have also been inves-
tigated in detail.
2. Materials and methods
2.1. Chemicals
Sodium chlorite (NaClO2, Sigma Aldrich, USA, 98%), acetate
buffer solution (pH ¼ 4.6, Sigma Aldrich, USA), 2,20 Azobis (Sigma
Aldrich, USA, 80%), and pure methyl methacrylate monomer (MMA,
Sigma Aldrich, USA, 99%) analytical reagents were used as received
without any further purification.
2.2. Fabrication of transparent wood
First, beech wood (BW) was cut into disc-shaped samples which
were rinsed with water. The rinsed wood pieces were then trans-
ferred to a box furnace for dehydration at 120  C for 24 h. The
dehydrated wood samples were then transferred to a solution
containing 5 wt % sodium chlorite in acetate buffer solution and
allowed to sit at 95  C for 12 h. This process bleached the wood and
removed lignin from the cell walls. The wood pieces were then
washed with deionized water. Later, these samples were washed
with ethanol, a solution of ethanol and acetone, and acetone so as
to remove any remaining water. The washed samples are referred
to as delignified wood (DW). Upon delignification, the samples
change from brown to white. The delignified wood samples were
stored in ethanol until further use. Later, the delignified wood
samples were impregnated with poly methyl methacrylate (PMMA)
by vacuum infiltration. The impregnation was performed for one
hour with three repetitions. Finally, the polymer-impregnated
wood was sandwiched between aluminum-wrapped glass slides
for heat treatment. The heat treatment was performed in a box
furnace at 85  C for 12 h. The heat-treated wood is labeled as
transparent wood (TW). A schematic of the fabrication process is
shown in Fig. 1.
2.3. Preparation of poly methyl methacrylate
PMMA was prepared by MMA monomer and 2, 20 Azobis initi-
ator. The initiator was 1 wt % of the monomer. The mixture of the
monomer and initiator was pre-polymerized at 90  C for 5 min. The
mixture was then cooled to room temperature in an ice-water bath
so as to terminate the polymerization.
2.4. Vacuum infiltration technique
To impregnate PMMA into the delignified wood with the help of
vacuum infiltration, a vacuum chamber and a vacuum pump. The
amount of vacuum pressure that is applied as well as the time of
vacuum infiltration, and stabilization of delignified wood plays a
vital role in the impregnation of PMMA into the delignified wood.
At first, to stabilize the wood in the vacuum chamber, the wood is
immersed in the PMMA solution. During the stabilization, i.e. when
the wood þ PMMA solution is under vacuum, the air that is present
in the pores of the wood is released as bubbles (shown in Fig. 1(b)).
An optimal time of an hour with three repetition at chamber
pressure of 0.1 bar has been chosen to completely remove the air
that is present inside the wood. Once, the wood þ PMMA solution is
stabilized, the chamber is disconnected from the vacuum pump
and is retained under vacuum. During this stage, the amount of
PMMA level that is immersed in the wood goes down which is
mainly because of the impregnation of PMMA into the wood.
Furthermore, PMMA hardens the wood and increases the ability to
stick to it. The PMMA impregnated wood is then further sand-
wiched in between the glass slides and further wrapped with
aluminum foil for heat treatment. The heat treatment is performed
in a box furnace at 85  C for 12 h. This heat-treated wood is then
labeled as transparent wood.
2.5. Characterization
The surface morphology of as-prepared wood samples was
measured by using an FEI Quanta 600 FEG scanning electron mi-
croscope. The non-conducting samples were coated with gold
before SEM measurements. Brunauer, Emmett and Teller (BET) ni-
trogen adsorption measurements were carried out on the beech
wood and delignified wood samples using a Micrometrics Gemini V
analyzer to determine their specific surface area. Before analyzing
the samples at 196  C by N2 physisorption, the samples were
degassed at 110  C for 24 h. At relative pressure ranging from 0.01 to
0.25, the data for all the samples were collected. Fourier transform
infrared spectroscopy (FT-IR) spectra was measured by using
attenuated total reflection (ATR) technique. The spectra were
recorded using a Varian 3100 FT-IR Excalibur. Spectral data were
collected over a range of 400 cm1 to 4000 cm1 by averaging 40
scans with a resolution of 8 cm1. The transmittance and haze
measurements were performed using a Lambda 950 UV/VIS NIR
spectrophotometer with a wavelength ranging from 300 nm to
850 nm. For haze experiment, an integrating sphere with three
ports, of which two of them are aligned to the sphere's center
allowing passage of the transmitted light through the center of the
sphere, was used for performing both measurements. ASTM stan-
dards - ASTM D1003 “Standard Method for Haze and Luminous
Transmittance of Transparent Plastics” was followed to measure
the percentage of haze in the samples [14]. The percentage of Haze
determined is given by,
 
T4 T3
Haze ¼   100 %
T2 T1
Where, T1, T2, T3, and T4 are the amount of transmission of the
 H.S. Yaddanapudi et al. / Vacuum 146 (2017) 649e654
Fig. 1. (a) Fabrication process of transparent wood, (b) vacuum Infiltration technique.
sample placement with respect to the integrating sphere i.e. T1 is
the transmission measured of a white standard present on the
reflectance port without any known sample at the first port.
Similarly, T2 is the transmission of a white standard on the reflec-
tance port with the sample on the first port, T3 is the transmission
without any sample along with an open reflectance port, and T4 is
the transmission with the sample on the first port along with
having an open reflectance port.
For practical applications mechanical characterizations were
also performed. The tensile tests for all the samples were carried
out using a tabletop Instron 5969. A cell load of 500 N along with a
strain rate of 1% per minute was utilized to carry out the tensile
measurements. The samples were tested at room temperature with
dimensions of 50 mm х 3 mm. The hardness of all the samples were
measured using Rockwell Hardness C-scale tester equipped with a
diamond indentor. A load of 60 kgf was used during the hardness
measurement. All the mechanical testing measurements were
performed at room temperature.
3. Results and discussion
3.1. Material characterization
Fig. 2 shows the SEM images of untreated beech wood (BW),
delignified wood (DW), and transparent wood (TW) at (a) low
magnification, and (b) high magnification. The SEM images show a
clear presence of the three-dimensional structure of the wood for
all the samples. Additionally, the SEM images of the beech wood
shows the presence of lignin along the pore walls of the wood. In
contrast to the untreated wood, the delignified wood shows that
651
even after delignification, the three-dimensional structure of the
wood is retained. Moreover, the pores are aligned in parallel to the
axis of the cells which indicate that the cellulose is still retained
even after delignification process.
In addition, the SEM images of the transparent wood showed
that the polymer has not only completely filled the pores present in
the wood, but is also in good contact with the cell walls. From these
observations, we believe that there is a strong interaction between
the polymer and cell walls of the wood which might be either
chemical or mechanical. Moreover, void spaces that could be
observed are mainly due to the shrinkage of methyl methacrylate
by volume after polymerization at the interface between the cell
wall of the wood and polymer [15].
Fig. 3 shows the FTIR analysis for untreated beech wood,
delignified wood, and transparent wood samples. It can be seen
that the absorption intensity at 3429 cm1 decreases from beech
wood to transparent wood. This decrease in intensity is due to the
reduction in the number of hydroxyl groups in the material. Thus,
because of the presence of the vinyl monomer, MMA is carrying an
ester group and an unsaturated C-C double bond. Upon polymeri-
zation, this gets grafted onto the wood matrix by its ester group
through the free-radical polymerization mechanism. As a result, a
chemical compounding exists between the polymer and the wood
matrix which results in the formation of wood-PMMA composite.
Furthermore, a new peak at 1732 cm1 and 800 cm1
e 900 cm1 is observed which corresponds to the carbonyl group of
the polymer, indicating that the polymer is grafted onto the wood
matrix, thus generating a strong chemical interaction as observed
in the SEM images of transparent wood shown in Fig. 2. Further-
more, the peak at 1232 cm1 present in the untreated wood
652 H.S. Yaddanapudi et al. / Vacuum 146 (2017) 649e654

Fig. 2. SEM images of untreated beech wood (BW), delignified wood (DW), and transparent wood (TW) at (a) low magnification, (b) high magnification.

corresponds to the lignin that is present in the sample. Apart from
the lignin bands, peaks at 3400 cm1 and 2927 cm1 were also
observed in all the samples, which are identified as O-H stretching
absorption and C-H absorption bands, respectively, for cellulose
and hemicellulose. In contrast to the untreated wood, the deligni-
fied wood shows the absence of lignin band which further confirms
that the lignin present in the wood is removed.
3.2. Optical measurements
Fig. 4 shows the optical transmittance measurements for un-
treated beech wood, delignified wood, and transparent wood of
varying thickness (0.3 mme0.7 mm) over a wide wavelength range
of 300 nme850 nm. It can be seen that the beech wood and
transparent wood exhibit almost 0% transmission. This is due to the
presence of cellulose, lignin and hemicellulose which absorb most
of the light [16]. In contrast to these, the optimized transparent
wood samples exhibited a transmission value as high as 70% above
500 nm. Moreover, as the thickness of the transparent wood varies,
the percentage of transmission also differs. For instance, from Fig. 4,
it could be comprehended that as the thickness of the sample in-
creases, the amount of transmission decreases. A maximum
transmittance of 70% was obtained for 0.1 mm thickness whereas a
minimum transmittance of 15% was obtained for 0.7 mm thick
 H.S. Yaddanapudi et al. / Vacuum 146 (2017) 649e654
Fig. 3. FTIR spectra of beech wood, delignified wood, and transparent wood over a
range of 400 cm1 to 4000 cm1.
transparent wood. This variation in the amount of transmittance is
due to the fact that when light gets transmitted, attenuation takes
place which is due to the absorption and scattering. Therefore, with
a higher thickness, light possess a longer pathway resulting lower
transmittance. The higher transmittance of transparent wood can
lead to the development of novel transparent wood windows when
compared to the plastic and glass windows.
Fig. 5 shows the optical haze measurements of transparent
wood with varying thickness and PMMA. A maximum optical haze
of about 49% was obtained for 0.7 mm thickness of the wood
sample above 400 nm. In contrast, the sample with a thickness of
0.3 mm exhibited a haze of only 18%. It is very important to control
and combine both the haze and percentage of transmittance for
various applications. For example, in the applications of display, a
haze of as low as 1%e15% is required to avoid glare [17]. On the
other hand, a haze of more than 15% is considered useful for ap-
plications such as solar cells. A high percentage of haze improves
the amount of light absorption efficiency of solar cells by increasing
the path of light that is being transmitted into the active layer. As a
result, there can be an enhancement in the short circuit current
Fig. 4. UV-Visible optical transmittance measurements of beech wood, delignified
wood, and transparent wood of varying thickness (0.1 mme0.7 mm) over a range of
300 nme850 nm.
653
density of solar cells. Based on this, our optimized transparent
wood samples, which show a high haze, can play an important role
as substrates for solar cell applications.
3.3. Mechanical testing
Fig. 6 shows the comparison of stress-strain curves for beech
wood, transparent wood, delignified wood, and PMMA. It is clearly
observed that the transparent wood is much stronger with an
elastic modulus is of 2.5 GPa than that of the delignified wood
whose elastic modulus is 2.1 GPa, beech wood of 1.52 GPa and
PMMA with an elastic modulus of 2.3 GPa. The low elastic modulus
of the delignified wood is due to the lack of strong hydrogen bonds
binding across the cell walls of the wood.
Furthermore, the transparent wood is harder whose hardness is
23 HRC when compared to the beech wood's 21 HRC, and
delignified wood's 12 HRC. This improved mechanical property of
the transparent wood is due to the enhanced interaction between
the polymer and the cell walls of the wood as observed in SEM
images shown in Fig. 1. Moreover, delignification of the wood re-
sults in enhancement of the specific surface area from 9.8 m2/g to
18.9 m2/g as determined by BET measurements. This enhancement
in the specific surface area facilitates the impregnation of PMMA
into the pores of the wood. As a result, a strong hydrogen bond is
formed between the polymer and the hydroxyl groups on the cel-
lulose across the cell walls. Therefore, this inter-cellulose-PMMA
bonding in transparent wood is expected to significantly improve
both the toughness and the hardness of the material.
4. Conclusion
In conclusion, we have reported the synthesis and character-
ization of optically transparent wood from beech wood as the
precursor material. The synthesis process includes two steps which
are mainly the delignification of the wood followed by vacuum
infiltration of polymer into the wood. SEM, and FTIR measurements
proved that the lignin is extracted out of the wood after delignifi-
cation and that the polymer is completely impregnated into the
wood. BET measurements performed on the untreated beech wood
and delignified wood indicated an increase in the specific surface
area which facilitates in the impregnation of PMMA into the
delignified wood. Optical measurements mainly optical trans-
mittance and transmittance haze performed showed a maximum
transmission of 70% and a haze of 49% over the wavelength of
500 nm. Additionally, the amount of haze tends to increase with
100
Transparent wood (t - 0.7 mm)
Transparent wood (t - 0.6 mm)
80 Transparent wood (t - 0.3 mm)
PMMA
% Haze
60
40
20
0
300 400 500 600 700 800
wavelength (nm)
Fig. 5. UV-Visible optical haze measurements of beech wood, delignified wood, and
transparent wood of varying thickness (0.3 mme0.7 mm) over a wide wavelength
range of 300 nme850 nm.
654 H.S. Yaddanapudi et al. / Vacuum 146 (2017) 649e654
Fig. 6. Stress v/s Strain relationship of beech wood, delignified wood, transparent
wood and PMMA.
increase in the thickness of the wood while that the optical
transmittance decreases with an increase in the thickness of the
wood. Mechanical testing consisted mainly of tensile test mea-
surements, and hardness measurements were performed proved
that the transparent wood exhibited enhanced mechanical prop-
erties when compared to that of the delignified wood. The high
transmittance and haze along with improved mechanical proper-
ties bestows transparent wood as a next generation material for
building sector and as substrates for solar cells.
Competing financial interests
The authors declare no competing financial interests.
Acknowledgments
Support from the NSF through Grant#1407650and 1234338 is
thankfully acknowledged.
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