Indian Journal of Engineering & Materials Sciences

Vol. 22, October 2015, pp. 534-540

Study of microstructure and mechanical properties of injection

molded Arboform parts
Dumitru Nedelcua*, Simona Plavanescu (Mazurchevici)a & Viorel Paunoiub
“Gheorghe Asachi” Technical University of Iasi, Blvd. Mangeron, No. 59A, 700050 Iasi, Romania
b
Department of Manufacturing Engineering, ”Dunărea de Jos” University of Galaţi, 800201, Romania
Received 31 January 2015; accepted 21 August 2015

The industry of petroleum-based plastic materials is one of the major responsible for numerous unpleasant
environmental impacts. The biggest negative effect is given by absence of plastics biodegradability and recyclability,
leading to accumulation of huge amount of waste. The experimental study is planed over the Taguchi methodology with two
levels and six input parameters. Experimental data show that the tensile strength reached 58.61±2.73 MPa at 23oC and
5.45±0.34 MPa at 60oC. The friction coefficient exhibits a slight decrease during the first 100 s, in case of disk rotation, and
then the value is stable throughout the whole testing. Considering disk oscillation, there is an increase in the friction
coefficient, which reaches a peak after about 50 s and then decreases within the range of 50-150 s. The material seems to
have a completely amorphous structure, without being able to accurately determine the type of existing constituents. It
includes C, O and other accompanying elements in very small proportions. The SEM analysis shows a randomly oriented
structure. In the chemical elements spectrum, carbon and oxygen predominate, in both percentage and atomic mass.
According to the analyses performed Arboform L, V3 Nature can replace plastic materials in many industries, such as
automotive, toys, construction, electrical, computers, mobile phone cases, etc.

Keywords: Amorphous materials, Mechanical properties, Scanning Electron Microscopy, X-ray diffraction, Injection
moulding

Materials are the main substances that have an
important effect on company development and require
some simple or complex manufacturing technologies.
The future use of recyclable materials will become an
extremely important factor in all fields of activity1. The
used material “liquid wood” – Arboform, is completely
biodegradable in the natural environment being a high-
quality thermoplastic engineering material for
applications that demand high technological standards.
Arboform behaves like any petrochemical plastic
material which means it can be heated and molded/
injected into a broad range of complex moldings using
standard injection equipment. It combines the positive
properties of natural wood with the processing
capabilities of thermoplastic materials2.
Therefore, “liquid wood”- Arboform, due to its
biodegradability and mechanical properties superior to
other plastics, and due to the fact that it can be reused
up to five times without affecting its mechanical
properties, could replace some plastics in the near
future. The technological injection parameters, such as
injection pressure, injection time, cooling time, mold
—————
*Corresponding author (E-mail: dnedelcu@tcm.tuiasi.ro)
temperature, etc., are different. Arboform L, V3 Nature
is composed of biopolymers such as lignin constituents
of wood and/or combination with other biopolymers
such as lignin derivatives of polylactide acid, etc.,
alkanoates polyhydroxy, used as binders for natural
fiber2,3. “Liquid wood” is much heavier than ordinary
plastics and the manufacture costs are nearly double
than those of polypropylene, the most common plastic
material. If taken into account the positive effects on
the environment, as compared to petroleum-derived
plastics, the benefits clearly outrun these
inconveniences. Samples obtained from “liquid wood”-
Arboform L, V3 Nature have great applicability in
different fields, such as ornaments, interior car parts,
connectors, switches, etc., electrical industry, mobile
accessories, computers, televisions, mobile phone
cases, etc.2,4,5
Experimental Procedure
The technical issue that the project consists in
obtaining of “liquid wood” samples through
monocomponent injection molding using SZ-600H
machine (Fig. 1), a process by means of which
 NEDELCU et al.: INJECTION MOLDED ARBOFORM PARTS 535

Fig. 1— (a) SZ-600H injection moulding machine and (b) machine working area with injected samples

products with characteristics superior to those made of Table 1—The levels value of input parameters
plastics are obtained. “Liquid wood”-Arboform grains
can be processed by mold injection, extrusion, Input parameter Ttop tinj tr Ss Pinj Tmat
(oC) (s) (s) (mm) (MPa) (o
C)
calendering, blow molding, deep drawing or pressing
into molded parts, half-finished product, sheets, film First level 165 9 18 60 80 50
soder profiles2,3,6. “Liquid wood” pellets, which are Second level 175 11 25 80 100 80
mainly composed of lignin discarded during the paper-
making process combined with cellulose and wood significant influence on the process is exercised by
waste from industrial plants are introduced in a bunker injection pressure followed by melt temperature and
where they are subjected to hot-air drying for two-four matrix temperature. These are followed by screw
hours, after which the pellets are transferred into the speed, injection time and cooling time, which are
bunker of an injection machine, from where the though less significant.
material enters an injection cylinder, electrically heated After the orthogonality and number of degrees of
at (165-175)°C, being afterwards injected into a mold, freedom conditions were analyzed7-9, there were
which is water cooled at a temperature of 23°C. The 16 experimental tests to be made. The values of the
main parameters of the “Liquid wood”-Arboform L, input parameters are shown in Table 1.
V3 Nature injection process which could be taken into A series of experiments were conducted to
account are melt temperature, mold temperature, demonstrate the reliability of this material and
injection rate, injection and holding pressure, cooling evaluate its potential for industrial applications.
time, holding pressure time inside the mould and Tensile test using Instron 3382, friction coefficient
injection time. using UMT-2 (CETR-Center of Tribology) and
The experiments were planned using the Taguchi flexural test using WDW 50E machine, were carried
methodology7. The model proposed by Viger and out to reveal its mechanical properties. The
Sisson8 is easy to be studied with the model of system microstructure was carry out on QUANTA 200 3D
comprising “I” factors: F1, F2 ... Fi each factor having ni Microscope and for XRD analysis was used the X'Pert
levels. Each experiment was conducted three times. Pro MRD Diffractometer.
The proposed matrix model takes into consideration six Results and Discussion
technological parameters with two levels (Table 1). The tensile tests were performed at room
The experimental research determined the coefficients temperature (RT-23oC) and 60°C respectively, using
of a type (1) model: a computer-controlled testing machine with a
constant crosshead speed of 5 mm/min according to
ZT = M + Ttop + tinj + tr + S s + Pinj + Tmat ISO 527-3: 2003 recommendations. For each testing
+ + PinjTtop + Pinj tinj + Pinj tr + Pinj S s + PinjTmat … (1)
temperature, many specimens were tensile tested to
determine the tensile strength and tensile strain at
where M is general average, Ttop is melt temperature tensile strength (engineering). All of the specimens
(oC), tinj is injection time (s), tr is cooling time (s), Ss is were prepared according to ISO 527-3: 2003
screw displacement (mm), Pinj is injection pressure recommendations to achieve type 1B test samples
(MPa), Tmat is matrix temperature (oC). The most
536 INDIAN J. ENG. MATER. SCI., OCTOBER 2015

(recommended for fiber-reinforced (thermo) A sliding speed of V=94.2 m/min and a friction
plastics). length of L=471m were calculated. The friction
Tensile strength coefficient caused by disk rotation (Fig. 3, curve 1)
Figure 2 shows the tensile results. Representative exhibits a slight decrease during the first 100 s, and
tensile stress vs. tensile strain curves were plotted to then the coefficient value is stable throughout the
reveal the homogeneity (uniformity) of mechanical whole testing time. The average friction coefficient
properties in case of all three samples tested (Fig. 1 using disk rotation is 0.1416. Considering disk
curves 1, 2 and 3). oscillation (Fig. 3, curve 2), during testing, there is an
Experimental data show that the tensile strength
reached 58.61±2.7 MPa at 23oC and 5.45±0.34 MPa
at 60oC. The tensile strain at tensile strength is
2.46±0.15% at 23oC and 60.02±6.16% at 60oC. The
total extension is 2.48±0.15% at 23oC and
83.96±10.68% at 60oC. Table 2 shows the total
extension, At (%), tensile strain at tensile strength, A
(%) and tensile strength, Rm (MPa) at 23oC, and the
Table 3 the same parameters at 60oC. The results
obtained are better than those obtained for PA12,
PVC, ABS, which are commonly used plastics10.

Friction coefficient
In order to use the materials, it is highly important
to know the constant of friction. Therefore, the
Universal UMT-2 (CETR-Center of Tribology, INC.
USA) pin-on-disk tribometer was used to determine
the tribological behavior of “liquid wood”-Arboform.
When choosing the tribosystem, the material couple
used for the manufacture of the components, the
friction conditions, the room temperature and
humidity play a very important role in testing. The
friction coefficient was determined in dry conditions
Fig. 2 — Tensile stress vs tensile strain at (a) 23oC and b) 60oC
by OL60 disk rotation and by its oscillation by an
180o angle11,12. The testing conditions were as Table 2—Statistic deviation of At, A and Rm at 23oC
follows: pressure force Fz=15 N, disk rotation n=60 Total Tensile strain at Tensile strength,
rpm, distance from disk rotation axis to pin-disk extension, tensile strength, (Rm), MPa
contact area r=15 mm, friction time t=300 s and (At ), % (A ), %
sample diameter 6 mm. The initial disk roughness was Sample 1 2.36 2.33 55.62
Ra=0.6 µm. Sample 2 2.44 2.42 59.25
The mathematical relations used to calculate the Sample 3 2.65 2.63 60.96
specific pressure, sliding speed and friction length are13: Media 2.48 2.46 58.61
StDev 0.15 0.15 2.73
Fz = p ⋅ A … (2)
Table 3—Statistic deviation of At, A and Rm at 60oC
T = L/v … (3)
Total extension, Tensile strain at Tensile strength,
(At), % tensile strength, (Rm), MPa
n = 30v / rπ … (4) (A), %
where p is the specific pressure (MPa), A is the Sample 1 74.86 66.83 5.34
contact area of pin-on-disk with a 6 mm diameter Sample 2 81.30 54.84 5.83
(mm2), v is the sliding speed (m/min) and r represents Sample 3 95.72 58.38 5.17
the radius testing (mm). Media 83.96 60.02 5.45
StDev 10.68 6.16 0.34
 NEDELCU et al.: INJECTION MOLDED ARBOFORM PARTS 537

increase in the friction coefficient, which reaches a

peak after about 50 s and then decreases within the
(50-150) s range. Further variation is similar, yet the
coefficient decreases. In this case, the average friction
coefficient is 0.1788. The variations of the friction
coefficient described do not include the noise
parameters.
For some industrial applications the friction
coefficient is important in terms of average size and
constant in time. The low values obtained for this
material lead to the idea of a smooth surface contact
friction resistance. The values read for the friction
coefficients are good as they indicate low friction as
compared to other plastic materials whose friction
coefficients values are higher, such as: PA66, PP, PE-
HD, ABS10.
Flexural tests
The flexural test measures the force required to
bend a beam under three point loading conditions.
The data are often used to select materials for parts
that will support loads without flexing. The flexural
modulus is used as an indication of a material’s
stiffness when flexed. Fig. 3 — The average variation of friction coefficient by (a) disk
rotation and (b) disk oscillation
The movement speed of the sleeper was 2 mm/min
and it was equivalent to the beam deflection variation.
The tests were conducted according to ISO 17814, on
specimens of 80×10×4 mm.
Figure 4 shows the general flexural test chart (a)
and load-deformation diagram (b) of the Arboform L,
V3 Nature. Were used three samples for flexural test
(1, 2, 3 curves for samples used). The low values of
the maximum arrow and deflection angle are
accounted for by the increased stiffness of the
material.
The modulus of elasticity may be determined after
tensile testing and also after flexural testing. In our
experimental research the value for modulus of
elasticity was 4330 MPa. Three specimens were used.
The values of the elasticity modulus obtained were
compared with some plastics values10. Thus, this
material, i.e. liquid wood, can replace a few plastic
materials such as: PA 66 (polyamide): 2830 MPa;
PA11 (polyamide): 3200 MPa; POM (acetal
homopolymer): 2620 MPa; PE-HD (high density
polyethylene):1400 MPa; PVDF (poly vinylidene
fluoride): 2000 MPa; ECTFE (etylene copolymer):
1700 MPa, if greater material stiffness is required.
Otherwise, when low stiffness is required, the liquid
wood can replace the following plastics: PA 66SF20 Fig. 4 — (a) The general scheme of flexural test and (b) load-
(polyamide black with 20% aramide fiber)-4800 MPa; deformation diagram
538 INDIAN J. ENG. MATER. SCI., OCTOBER 2015
PEEK GF 30 (poly ether ether ketone with 30% glass
fiber)-9200 MPa; PEEK CF 30 (poly ether ether ketone
with 30% carbon fiber)-18800 MPa; PEK (poly ether
ketone with 10% glass fiber, 10% graphite and 10%
PTFE)-11500 MPa; PAI (polyamide imide)-5000 MPa;
PPS GF 40 (poly phenylene sulphide with 40% glass
Fig. 5 — XRD analysis (a) at the end of sample and (b) in fracture
surface
Fig. 6 — SEM image obtained with secondary electrons (SE) (a) at the end of sample and (b) in fracture surface
fiber)-13000 MPa; PEI GF 30 (poly ether imide with
30% glass fibre)-9000 MPa; PVDF CF 20 (poly
vinylidene fluoride with 20% glass fiber)-6000 MPa.
XRD analysis
It was used the X'Pert Pro MRD Diffractometer
and X’pert HighScore Plus software produced by
PANalytical for XRD analysis. The image
obtained with this analysis is shown in Fig. 5. The
scan was made on a 5 mm segment at a 2θ distance
between (0-59.9932°). According to the
diffractogram, the material seems to have a
completely amorphous structure, without being
able to accurately determine the type of existing
constituents. It includes C, O and other
accompanying elements in very small proportions.
In the light of the facts above, it is also impossible
to determine network parameters and network
type. Analysis was performed in two cases, at the
end of the sample (Fig. 5a) and in the fracture
surface (Fig. 5b).
SEM analysis
An electronic QUANTA 200 3D Microscope was
used for scanning electron microscopy (SEM)
analysis, which works with double electron and ion
beam (Fig. 6). The image was obtained taking into
account the following parameters: the 10 kV
accelerating voltage (HV) of the secondary electrons
(SE); a 1400X magnification (mag); a 15.1 mm
working distance (WD); a large field detector
(LFD) used for the analysis of the non conductive
samples (polymers, textile fibers, powders etc.); a
0o tilt angle (tilt); a 60P pressure inside the
microscope room. SEM was conducted at the end of
 NEDELCU et al.: INJECTION MOLDED ARBOFORM PARTS 539

the sample and in the fracture surface using a 300 the chemical elements range is shown in Fig. 7a, at
µm scale. SEM analysis shows an even randomly the end of the sample on a 304 s range acquisition
oriented structure. time, and in the Fig. 7b, in the fracture surface. The
EDAX analysis sample surface used for quantitative chemical element
Energy dispersive X-ray spectroscopy (EDAX) is analysis with X-ray in SEM was also described.
an analytical technique used for elemental analysis or Table 4 shows the weight and atomic percentages of
chemical characterization of a sample. An electronic the chemical elements and also the ZAF correction
QUANTA 200 3D microscope which works with (Z-atomic number correction, A-sample matrix
double electron and ion beam and with EDAX absorption correction, F-correction of secondary
Genesis software was used for measurement. Thus, X-ray emission) for the sample obtained at the end,
Table 4—The weight, atomic percentages for chemical elements Table 5—The weight, atomic percentages for chemical elements
and ZAF correction (at the end of the sample) and ZAF correction (in fracture surface)
Element Weight percentages, Atomic percentages, Element Weight percentages, Atomic percentages,
(Wt), % (At), % (Wt), % (At), %
CK 42.51 50.46
CK 41.29 48.71 OK 53.70 47.86
OK 57.08 50.56 NaK 00.98 00.61
NaK 00.32 00.20 SiK 00.36 00.18
SiK 00.31 00.15 SK 00.22 00.10
SK 00.11 00.05 ClK 00.86 00.35
ClK 00.29 00.12 KK 00.37 00.13
KK 00.20 00.07 CaK 00.59 00.21
CaK 00.40 00.14 FeK 00.42 00.11
Matrix Correction ZAF Matrix Correction ZAF

Fig. 7 — Spectrum of chemical elements and surface used (a) at the end of the sample and (b) in the fracture surface
540 INDIAN J. ENG. MATER. SCI., OCTOBER 2015
where Table 5 shows the results of the analysis in the
fracture surface. Was highlighted the main chemical
elements depending on the relative energy peaks.
Conclusions
“Liquid wood”-Arboform L, V3 Nature may
replace plastic materials in the near future, since it is
a recyclable and biodegradable material. The
experimental research followed a Taguchi plan with
six input parameters each of them with two levels.
Experimental data concerning the tensile strength,
flexural test and friction coefficient leads to the idea
that Arboform L, V3 Nature can replace some plastic
materials such as: PA66, PP, PE-HD, ABS, PA,
POM, PVDF, ECTFE, PA 66SF20, PEEK GF 30,
PEEK CF 30, PEK, PAI, PPS GF 40, PEI GF 30,
PVDF CF 20.
After analyzing the diffractogram, it can be
noted that the material seems to have a completely
amorphous structure, without being able to
accurately determine the type of existing
constituents. It includes C, O and other
accompanying elements in very small proportions.
In the light of the facts above, it is also impossible
to determine network parameters and network type.
The SEM analysis shows an even randomly
oriented structure. In the chemical elements
spectrum, carbon and oxygen predominate, in both
percentage and atomic mass, followed by Na, Si, S,
Cl, K and Ca. According to the results obtained and
to the conclusions drawn, “liquid wood”-Arboform
L, V3 Nature can replace plastic materials in many
industrial applications, such as: ornaments,
including for cars, connectors, switches etc.,
electrical industry, different mobile accessories,
computers, televisions, mobile phone cases, etc.
Acknowledgment
This work was supported by the strategic grant
POSDRU/159/1.5/S/133652, co-financed by the
European Social Fund within the Sectorial
Operational Program Human Resources Development
2007-2013.
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