Synthesis and Characterization of Bio-based Nanomaterials from Jabon (Anthocephalus cadamba (Roxb.) Miq) Wood Bark: an Organic Waste Material from Community Forest

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The application of nanotechnology to produce nanomaterials from renewable bio-based materials, like wood bark, has great potential to benefit the wood processing industry. To support this issue, we investigated the production of bio-based nanomaterials using conventional balls milling. Jabon (Anthocephalus cadamba (Roxb.) Miq) wood bark (JWB), an organic waste material from a community forest was subjected to conventional balls milling for 96 h and was converted into bio-based nanomaterial. The morphology and particle size, chemical components, functional groups and crystallinity of the bio-based nanomaterial were evaluated using scanning electron microscopy (SEM), scanning electron microscopy extended with energy dispersive X-ray spectroscopy (SEM-EDS), Fourier transform infrared spectroscopy (FTIR), and X-ray diffraction (XRD). The particle-sizes obtained for the JWB bio-based nanomaterial were between 43 nm to 469 nm and the functional groups were detected as cellulose. The chemical components found were carbon, oxygen, chloride, potassium and calcium, except for the sample produced from sieve type T14, which did not contain chloride. The crystalline structure was calcium oxalate hydrate (C2CaO4.H2O) with crystalline sizes 21 nm and 15 nm, produced from sieve types T14 and T200 respectively.

본문

J. Math. Fund. Sci., Vol. 47, No. 2, 2015, 205-218           205

# Synthesis and Characterization of Bio-based Nanomaterials from Jabon ( Anthocephalus cadamba (Roxb.) Miq) Wood Bark: an Organic Waste Material from Community Forest

Sutrisno 1 *, Tati Suryati Syamsudin 1 , Eka Mulya Alamsyah 1 &

Bambang Sunendar Purwasasmita 2

1School of Life Sciences and Technology, Institut Teknologi Bandung
2Faculty of Industrial Technology, Institut Teknologi Bandung
Jalan Ganesha No. 10, Bandung 40132, Indonesia

*Email: sutrisno@sith.itb.ac.id

Abstract. The application of nanotechnology to produce nanomaterials from
renewable bio-based materials, like wood bark, has great potential to benefit the
wood processing industry. To support this issue, we investigated the production
of bio-based nanomaterials using conventional balls milling. Jabon
( _Anthocephalus cadamba_ (Roxb.) Miq) wood bark (JWB), an organic waste
material from a community forest was subjected to conventional balls milling for
96 h and was converted into bio-based nanomaterial. The morphology and
particle size, chemical components, functional groups and crystallinity of the
bio-based nanomaterial were evaluated using scanning electron microscopy
(SEM), scanning electron microscopy extended with energy dispersive X-ray
spectroscopy (SEM-EDS), Fourier transform infrared spectroscopy (FTIR), and
X-ray diffraction (XRD). The particle-sizes obtained for the JWB bio-based
nanomaterial were between 43 nm to 469 nm and the functional groups were
detected as cellulose. The chemical components found were carbon, oxygen,
chloride, potassium and calcium, except for the sample produced from sieve type
T14, which did not contain chloride. The crystalline structure was calcium
oxalate hydrate (C2CaO4.H2O) with crystalline sizes 21 nm and 15 nm, produced
from sieve types T14 and T200 respectively.

Keywords: _bio-based nanomaterial; community forest; conventional balls milling;_
_Jabon wood bark; organic waste material._

1 Introduction

Wood from community forests is a good substitute for natural forest wood and
is beneficial for the diversification of raw materials in the wood processing
industry. A high potential of community forests is located on Java Island (55.73
million m 3 ) with a total area of 1.94 million hectare (ha) and a potential average
of 28.73 m 3 /ha. In West Java particularly, the area of community forests reaches

Received March 18 th, 2014, 1 st Revision March 2014, 2 nd Revision 7 th May 2014, 3 rd Revision 10 March 2015,
Accepted for publication 30 April 2015.
Copyright © 2015 Published by ITB Journal Publisher, ISSN: 2337-5760, DOI: 10.5614/j.math.fund.sci.2015.47.2.7

206 Sutrisno, _et al._

419,041.93 ha, with a timber potential of 12,005,551 m 3 or potential average of
28.65 m 3 /ha. There are at least 32 species of woods [1].

The high economic potential of community forest timber in West Java can lead
to the improvement of the people’s economical situation. However, in order to
obtain maximum benefit from the community forests it is not enough to simply
make use of the timber. Alternative uses for the wood bark waste must also be
developed. The wood bark volume can be estimated based on the wood volume,
which ranges from 9-15% [2] to 10-25% [3]. Assuming an average wood bark
volume of 10% and the area of community forests in West Java reaching
419,041.93 ha with a potential average of 12,005,551 m 3 [1], the production of
wood bark waste would be about 1,200.55 m 3 . In addition, wood bark waste
could also have great economic potential for wood processing industries due to
the large variety and high volume of wood processed. Currently, wood bark
waste is mostly used in wood processing industries as a fuel source for boilers
to produce steam for the drying process. Wood bark could also be used for
many other purposes, such as filler material for adhesive formula [4-6]; certain
species of wood bark containing condensate tannins can be made into tannin
adhesive [7-11] or wood preservative [12-14].

According to Allouche [15], organic nanoparticles can be described as solid
particles composed of organic compounds, ranging in diameter from 10 nm to
1000 nm. Bio-based nanomaterials can be defined as organic materials that have
structured components of at least one dimension less than 1000 nm. In future
nanotechnology research efforts, bio-based nanomaterials have a great potential
for improving the forest processing industry in the form of coatings, biocides or
modified resins [16]. This is due to the tendency of consumers, industry and the
government to increasingly look towards products with raw materials derived
from renewable natural resources that are sustainable, biodegradable and nonpetroleum based, and have a small negative impact on the environment, animals
and human health [17]. Besides that, bio-based nanomaterials lead to the
emergence of new high-value bio-product applications [18].

The objective of this research was to produce bio-based nanomaterial from
Jabon ( _Anthocephalus cadamba_ (Roxb.) Miq) wood bark (JWB) using
conventional balls milling. The bio-based nanomaterial obtained from JWB was
characterized using scanning electron microscopy (SEM), scanning electron
microscopy extended with energy dispersive X-ray spectroscopy (SEM-EDS),
Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD)
according to Abdul Khalil, _et al_ . [19] and Purwasasmita, _et al._ [20,21].

Bio-based Nanomaterials from Jabon Wood Bark 207

2 Materials and Methods

2.1 Preparation of Wood Bark Powder

Jabon wood bark (JWB) was collected from the community forest in Cibugel
district, Sumedang regency, West Java province, Indonesia. Geographically, the
sampling site is located at 6°44 ’ -70°83 ’ south latitude and 107°21 ’ -108°21 ’ east
longitude. The JWB taken from the community forest was cut using a cleaver
and broken into small pieces (2 x 2 cm 2 ), solar dried until the moisture content
was less than 5%, and made into powder by pounding it using a pestle, and
sieved by 60-mesh sieve.

2.2 Synthesis of Bio-based Nanomaterials

In the first stage, 0.25 kg of the wood bark powder (60 mesh) was further
ground by using a conventional balls mill for 48 h at 100 rev min -1 with a ratio
weight of alumina balls to powder 2.9:1. In the second stage, the wood bark
powder was treated with liquid nitrogen with a ratio volume of liquid nitrogen
to powder 2:1, then ground using a conventional balls mill for 48 h under the
same conditions as in the first stage. The wood bark powder was then filtered by
a single sieve equipped with screen printing fabric type T14. For further
evaluation, the wood bark powder was filtered again by four sieves equipped
with screen printing fabric types T77, T90, T120 and T200 respectively.

The milling container was made of PVC pipe with a diameter of 10.16 cm and a
length of 27.3 cm. The balls were made of alumina with a diameter size of 1.34.0 cm. Figure 1 shows a schematic diagram of the synthesis of bio-based
nanomaterial using conventional balls milling.

Figure 1 Schematic diagram of the synthesis of bio-based nanomaterial using
conventional balls milling.

208 Sutrisno, _et al._

2.3 Characterization of Bio-based Nanomaterial

The morphology and diameter of the bio-based nanomaterial from JWB was
characterized using SEM (JEOL-JSM-6510LV SEM type). Samples were taken
and coated with platinum using an ion sputter coater. SEM analysis was
extended to obtain the elemental composition of the JWB by means of energy
dispersive X-ray spectroscopy analysis (SEM-EDS).

A Fourier transform infrared spectroscope (FTIR), Prestige 21, Shimadzu
(Japan) was used to examine the functional groups present in the JWB. Five mg
of samples were mixed with 160 mg KBr (1:32). They were then pressed into
transparent thin pellets. An FTIR spectrum of the JWB was obtained in the
range of 4500-500 cm −1 . The spectral output was recorded in the transmittance
mode as a function of wave number.

The crystalline structure of the organic bio-based nanomaterial produced from
JWB was identified using a powder X-ray diffraction instrument (XRD, PW
1710, Philips analytical), operating at 40 Kv and 30 mA with Cu/Kα (λ =
1.54060 °A) radiation source. The diffractrograms were scanned using a
scanning rate of 0.5° s -1 in steps of 0.02° from 5° to 65° (2 _θ_ ) at room
temperature. The crystalline size was determined from the X-ray diffraction
peaks using Scherrer’s equation [22] as follows:

_D_ = _K_ λ / β cos θ (1)

where _D_ is the diameter of the crystalline size; _K_ is the shape factor with a value
of 0.9-1.4 or Scherrer’s constant of the order of unity for usual crystals; λ is the
wavelength of the X-rays (1.54060 Ǻ); β is the value of the _full width at half_
_maximum_ (FWHM); and θ is the diffraction angle. XRD patterns were identified
using the PDF2 CD-ROM (JCPDS-International Centre for Diffraction Data).

3 Results and Discussion

3.1 Diameter Size of Bio-based Nanomaterial

The diameter sizes of the particles from SEM analysis were 140-469 nm, 94108 nm, 69-98 nm, 52-84 nm, and 43-57 nm produced from sieve types T14,
T77, T90, T120 and T200 respectively with magnifications of 20,000-30,000
times. The morphology shows the formation of agglomerates among the
particles (Figure 2). Therefore, the particles from the organic material of JWB
can be considered nanoparticles since their size is in the range of 10-1000 nm

[15]. The proportions of the nanoparticle sizes were 28.40%, 21.97%, 10.99%
and 1.04% produced from sieve types T77, T90, T120 and T200 respectively

Bio-based Nanomaterials from Jabon Wood Bark 209

and the (37.61%) remaining nanoparticles were retained from sieve type T77
(Table 1).

Table 1 Sieve types and nanoparticles sizes.

Nominal sieve

opening
(microns)

Particles
size (nm)

Sieve

type

Sieve
designation

(mesh)

Proportion

Remark
(%)

T14
T77

95 151**) 140-469 - Single sieve
523 28**) 94-108 28.40

T90 611 24**) 69-98 21.97
T120 815 18**) 52-84 10.99
T200 1358 10.6*) 43-57 1.04
37.61 Retained on
sieve type T77
Note : *) based on SEM analysis; **) based on conversion from T200 sieve type

Figure 2 SEM analysis of JWB produced from sieve type T77.

3.2 Chemical Components of Bio-based Nanomaterial

Figure 3 shows the energy dispersive X-ray spectroscopy analysis (EDS)
spectra with the chemical composition of JWB. An essential observation is that
all JWB nanoparticles produced from sieve types T77, T90, T120 and T200
contained carbon, oxygen, chloride, potassium and calcium. However, the
sample produced from sieve type T14 contained only carbon, oxygen,
potassium and calcium. For comparison, pine wood bark contains phosphorous,
potassium, manganese, copper, calcium, magnesium, and zinc [23]. This
corresponds with the nutrient content of wood bark differing between species,
tree age, environmental factors, and growing site [23]; it contains about 60-70
percent glucose [2].

210 Sutrisno, _et al._

(a)

(b)

Figure 3 EDS analysis of JWB produced from (a) T14 and (b) T77 sieve type.

Bio-based Nanomaterials from Jabon Wood Bark 211

3.3 Functional Groups of Bio-based Nanomaterial

The FTIR spectra of the JWB with diameters 140-469 nm, 94-108 nm, 69-98
nm, 52-84 nm, and 43-57 nm produced from T14, T77, T90, T120 and T200
sieve types respectively are similar, as illustrated in Table 2 and Figure 4. They
are composed of cellulose, the main constituent in the cell wall of natural fibers

[24-27].

In addition, the FTIR analysis shows the presence of a C=O stretching band at
1724 cm -1 in the nanoparticles of the JWB produced from sieve types T77 and
T90 (Figure 4(b) and 4(c)) and a C=O stretching band at 1732 cm -1 of the JWB
produced from sieve type T200 (Figure 4(e)), while no such structures were
observed in the nanoparticles of the JWB produced from sieve types T14 and
T120 (Figure 4(a) and Figure 4(d)). This result implies that the balls milling
changed the presence of the functional groups of cellulose. Abdul Khalil, _et al_ .

[19] reported that the silanol (Si-OH) functional group was present after the oil
palm ash was milled with high-energy ball milling for 30 h, due to the balls
milling effect.

Table 2 Infrared spectrum of JWB.

Sieve types and peak wave number (cm ~~-1~~ ) Assign

Sieve types and peak wave number (cm ~~-1~~ ) Assign Reff.

T14 T77 T90 T120 T200 ment
3342-3368 3412-3356 3408-3352 3379 3383-3375 OH [24,25,
stretching 27,28]

ment

[24,25,

stretching 27,28]

2920-2850 2922-2852 2922-2852 2924-2856 2922 CH
stretching
2362-2343 - - - - OH
stretching

- 1724 1724    - 1732 C=O
stretching
1622 1624 1625 1624 1627 COO [26, 27]
stretching

[26, 27]

1525 1514 1517 1519 1508 C=C
stretching

[24, 25,

[26]

stretching 28]

1429-1259 1435-1257 1435-1257 1436-1257 1429-1249 C-H [26]
wagging

1153 1155 1155 1153 1157 C-C ring
breathing,
asymmetric

[25, 28]

1103-1028 1103-1031 1103-1031 1029 1105-1055 C-O-C
glycosidic
791-526 779-524 779-526 777-526 773-530 C-OH outof-plane
bending

[24]

Note : – = no data

212 Sutrisno, _et al._

(a)

4500 4000 3500 3000 2500 2000 1750 1500 1250 1000 750 500

jt77 1/cm

(b)

Figure 4 _Continued._ FTIR analysis of JWB produced from five sieve types: (a)
T14, (b) T77, (c) T90, (d) T120 and (e) T200.

Bio-based Nanomaterials from Jabon Wood Bark 213

4500 4000 3500 3000 2500 2000 1750 1500 1250 1000 750 500

jt90 1/cm

(c)

4500 4000 3500 3000 2500 2000 1750 1500 1250 1000 750 500

jt120 1/cm

(d)

Figure 4 _Continued._ FTIR analysis of JWB produced from five sieve types: (a)
T14, (b) T77, (c) T90, (d) T120 and (e) T200.

214 Sutrisno, _et al._

4500 4000 3500 3000 2500 2000 1750 1500 1250 1000 750 500

jt200 1/cm

(e)

Figure 4 FTIR analysis of JWB produced from five sieve types: (a) T14, (b)
T77, (c) T90, (d) T120 and (e) T200.

3.4 Crystallinity of Bio-based Nanomaterial

As comparison of crystalline size, the crystallinity was studied from the biobased nanomaterial with the largest and smallest nanoparticle size, produced
from sieve types T14 and T200 respectively. The crystalline structure was
explained by the presence of peaks after the samples were scanned using X-ray
in a range of diffraction angles. The XRD analysis (Figure 5) shows the
crystalline structure of calcium oxalate hydrate (C2CaO4.H2O). This
is due to the essential chemical composition of the bio-based
nanomaterial, consisting of carbon, oxygen, chloride, potassium and calcium,
except for the sample produced from sieve type T14 (which contained no
chloride). In a previous research, hexagonal calcium oxalate crystals were also
obtained from bark of basswood ( _Tillia americana_ ) [27]. The reflecting peaks at
2 θ = 14.94°, 24.44°, 30.14° and 38.32° were used to estimate the average
crystalline size produced from sieve type T14, which was calculated to be 21
nm (Figure 5(a)). The reflecting peaks at 2 θ = 14.98°, 20.27°, 22.92°, 24.36°
and 29.48° were used to estimate the average crystalline size produced from
sieve type T200, which was calculated to be 15 nm (Figure 5(b)). Crystallinity
is one of several factors that affect the accessibility of cellulose; other factors

Bio-based Nanomaterials from Jabon Wood Bark 215

are contents and distribution of lignin and hemicellulose, porosity, and particle
size [29].

(a)

(b)

Figure 5 XRD analysis of JWB produced from (a) T14 and (b) T200 sieve type.

4 Conclusions

Bio-based nanomaterial from Jabon wood bark was produced using
conventional balls milling with a diameter of about 140-469 nm, 94-108 nm,
69-98 nm, 52-84 nm and 43-57 nm from sieve types T14, T77, T90, T120 and
T200 respectively. It is concluded that the particles of the bio-based material
from JWB can be considered nanoparticles since their size is in the range of 101000 nm.

The chemical composition of the JWB contained carbon, oxygen, chloride,
potassium, and calcium, except for the sample produced from sieve type T14,
which did not contain chloride. The functional groups that exist in the JWB
were detected as cellulose. Additionally, conventional balls milling changed the
presence of functional groups of JWB’s cellulose.

The crystalline structure of the bio-based nanomaterial produced from JWB was
calcium oxalate hydrate (C2CaO4.H2O) with crystalline size 21 nm and 15 nm

216 Sutrisno, _et al._

produced from sieve types T14 and T200 respectively.

Acknowledgments

The authors would like to thank all reviewers of the manuscript, among others
Dr. Ahmad Faizal for his comments and correction. We would like to also thank
Prof. Dr. Bambang Sunendar Purwasasmita (Head of the Advanced Material
Processing Laboratory), Engineering Physics Department, Faculty of Industrial
Technology, Institut Teknologi Bandung (ITB) for providing research facilities;
Board of Research and Community Services, ITB, and the Ministry of
Education and Culture of Republic of Indonesia for financial support for this
research through the Decentralization Research Program, year 2013, and the
Dean of ITB graduate school for her policy to provide the editing service to
revise the English writing of this research paper.

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