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 1st Annual Applied Science and Engineering Conference IOP Publishing
IOP Conf. Series: Materials Science and Engineering 180 (2017) 012012 doi:10.1088/1757-899X/180/1/012012

International Conference on Recent Trends in Physics 2016 (ICRTP2016) IOP Publishing

Journal of Physics: Conference Series 755 (2016) 011001 doi:10.1088/1742-6596/755/1/011001

The Mechanical Properties and Microstructure Characters of

Hybrid Composite Geopolymers-Pineapple Fiber Leaves (PFL)

N Amalia*, S Hidayatullah, Nurfadilla, Subaer

Laboratorium Fisika Material, Jurusan Fisika, Universitas Negeri Makassar, Indonesia
Jl. Daeng Tata Raya, Makassar, Indonesia

*[email protected]

Abstract. The objective of this research is to study the influence of organic fibers on the
mechanical properties and microstructure characters of hybrid composite geopolymers-
pineapple fibers (PFL). Geopolymers were synthesized by using alkali activated of class C-fly
ash added manually with short pineapple fiber leaves (PFL) and then cured at 60ºC for 1 hour.
The resulting composites were stored in open air for 28 days prior to mechanical and
microstructure characterizations. The samples were subjected to compressive and flexural
strength measurements, heat resistance as well as acid attack (1M H 2SO4 solution). The
microstructure of the composites were examined by using Scanning Electron Microscopy-
Energy Dispersive Spectroscopy (SEM-EDS). The measurement showed that the addition of
pineapple fibers was able to improve the compressive and flexural strength of geopolymers. The
resulting hybrid composites were able to resist fire to a maximum temperature of 1500ºC. SEM
examination showed the presence of good bond between geopolymer matrix and pineapple
fibers. It was also found that there were no chemical constituents of geopolymers leached out
during acid liquid treatment. It is concluded that hybrid composite geopolymers-pineapple fibers
are potential composites for wide range applications.

1. Introduction
The term of hybrid composite implies material contained more than one type of material such as organic
fibers which act as reinforcement [1]. This has a potential to provide improved properties such as
toughness, strength and ductility, and fire resistance [2]. Basically, composite comprise of two parts,
matrix and aggregate. In recent years, organic fibers have received numerous attention due to their
excellent properties such as high tensile and compressive strength, and difficult to crack [3]. Organic
fiber used in this research is pineapple fiber extracted manually from pineapple leaves. Pineapple is a
well-known fruit all over the world. Pineapple leaves have attracted global attention because it creates
environmental problems. New efforts are needed to overcome the environment impact due to the
abundance of pineapple leaves dumped on the ground especially around the traditional markets. In recent
years, for example, pineapple leaves have been used in the production of rough textile [4]. The addition
of fibers as aggregate in the production of composite is intended to reduce the volume of the matrix [5].
Besides that, fibers show good adhesion properties and capable to control micro crack along the matrix
[3]. Pineapple fibers have high cellulose and it is known that the quality of fibers depends on the amount
of cellulose [4, 6]. The tensile strength of pineapple fiber is about 1088.60 MPa and its modulus Young
is around 6441,6 GPa [7]. The length and the content of fiber in composite were found to increase the
tensile and the impact strength of the material [8]. Other study showed that pineapple fiber leaves (PFL)
exhibited superior mechanical properties due to its nature high-cellulose content and relatively low

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 1st Annual Applied Science and Engineering Conference IOP Publishing
IOP Conf. Series: Materials Science and Engineering 180 (2017) 012012 doi:10.1088/1757-899X/180/1/012012

micro-fibrillar angle (14o) [9]. The matrix used in this study was geopolymer synthesized trough alkali
activated fly ash (class-C). Geopolymers have a potential for a wide variety of applications, whether use
pure, with fillers or reinforced [10]. A number of research have utilized fly ash as matrix and inorganic
fibers as aggregate in the production of geopolymer composite (particularly concretes) and reported
good mechanical properties, low thermal conductivity and high fire resistance [11, 12, 13].

2. Experimental Method
Geopolymers paste were synthesized by using class-C fly ash activated with alkaline solution. The molar
ratio of the mixture were SiO2/Al2O3 = 3.0, Na2O/SiO2 = 0.2, and H2O/N2O = 10.0. Pineapple fiber
leaves (PFL) was extracted manually and soaked into 0,5M NaOH for 1 hour, dried and cut to about 5.0
mm in length. The composites were produced by varying the mass of aggregate relative to the mass of
fly ash with a variation of 0%, 0.2%, 0.4%, 0.6%, 0.8% and 1.2%. The mixture of geopolymer paste and
PFL was molded and cured at 60ºC/1 hour. The resulting materials were demolded and left in open air
for 28 days before conducting any measurements. The size and the shape of the sample were customized
in accordance with the measurement and characterization requirement such as flexural strength, fire
resistance, acid attack, and SEM-EDS.
The compressive strength of the samples were measured by using universal testing machine with a
maximum load of 50 ton, and the flexural strength was measured by using three bending flexural
strength method. The level of crystallinity and chemical compositions of fly ash were measured by using
Rigaku Mini Flex II X-Ray Diffraction operated at 30 kV and scan speed 0.2o/s. The morphology and
the element compositions of fly ash was observed by using Tescan Vega 3 SB Scanning Electron
Microscope couple with Bruker Energy Dispersive Spectrometer (EDS). The fire resistance of the
composite was examined by exposing the sample surface on fire for 20 – 30 minutes and measured the
temperature around 2.0 cm from the fire spot by using a thermocouple. The acid resistance of the samples
was measured by immersing the sample into H2SO4 solution for 7 days.

3. Result and Discussion

Figure 1. Shows the sample of hybrid composite PFL-geopolymers with a size of (6.0 x 3.0 x 3.0) cm
produced in this study. Physically, the sample appear glossy and no apparent cracks observed on the
surfaces of the samples.

Figure 1. Example of hybrid composite geopolymers-PFLproduced in this study.

Figure 2 (a) and (b) shows the SEM image and diffractogram of fly-ash, respectively. The image
shows the spherical shape of fly ash morphology with a particle size smaller than 10 µm. The size of fly
ash particles suggest that its surface area is large and hence the reactivity of fly ash and sodium silicate

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 1st Annual Applied Science and Engineering Conference IOP Publishing
IOP Conf. Series: Materials Science and Engineering 180 (2017) 012012 doi:10.1088/1757-899X/180/1/012012

solution is high. The diffractogram showed that the crystallinity level of fly ash is fairly high and the
main chemical compositions of fly ash were quarts, magnesium, iron diiron magnetite and calcium
peroxide. The wt% of elements and oxides of fly ash were examined by using Energy Dispersive
Spectroscopy (EDS) as shown in table 1.

(a) (b)
Figure 2. SEM image (a), and X-ray diffraction pattern (b) of fly ash used in this study

Table 1. The wt% of elements and oxides of fly ash measured with EDS

No Element Atom (at. %) Compound norm. wt %

1 Oxygen 58.50 0.00
2 Sodium 0.76 Na2O 0.99
3 Magnesium 3.65 MgO 6.20
4 Aluminium 10.36 Al2O3 22.25
5 Silicon 11.89 SiO2 30.10
6 Sulfur 0.15 SO3 0.51
7 Potassium 0.70 K2O 1.39
8 Calcium 5.90 CaO 13.95
9 Titanium 0.36 TiO2 1.20
10 iron 7.73 FeO 23.41

Table 1 shows that the molar ratio of SiO2 and Al2O3 is in the range of good geopolymers production.
The high content of CaO however make the geopolymers paste to set in a very short time and difficult
to control in large quantity.
Table 2 shows the results of mechanical measurements of the resulting composites. It can be seen
that the density of geopolymers paste was around 2,02 g/cm3 and slightly decrease as the mass of fibers
increases. The magnitude of compressive strength increase as the concentration of fibers increase.
However, as the mass of fibers reached 1.2% relative to the mass of fly ash the bond between the matrix
and the fibers weaken and as a result the compressive strength decrease significantly as in sample NN
04. The flexural strength of all composites increase as the mass of the fiber increase. This is
understandable since the presence of fibers will enhance the ability of the geopolymer matrix to resists
external load by sharing the stress-strain with the fibers.

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 1st Annual Applied Science and Engineering Conference IOP Publishing
IOP Conf. Series: Materials Science and Engineering 180 (2017) 012012 doi:10.1088/1757-899X/180/1/012012

Table 2. The average value of density, compressive and flexural strength of the samples.

Density Compressive Strength Flexural Strength

NO Sample
(g/cm3) (MPa) (MPa)
1 NN 01 2.02 23.33 6.00
2 NN 02 1.97 41.57 6.83
3 NN 03 1.97 58.24 7.07
4 NN 04 1.99 25.20 7.09

Fire resistance measurement was conducted by using flame torcher and a thermocouple was inserted
around 2.0 cm from the flame spot (Figure 3) to register the temperature as a function of time. The
temperature of the flame used can reach 1500ºC and the sample was exposed to fire for 30 minutes. The
measurement was conducted to investigate the ability of geopolymers matrix to protect the organic fibers
from intense fire or heat.

Figure 3. Fire resistance measurement on the surface of the composite

The rise of the temperature at the point 2.0 cm from the fire spot was monitored every 2 minutes.
Figure 4 shows the graph of temperature as a function of time for the fire source (a) and the temperature
of the sample surface.
2000

a
temperature (oC)

1500

1000

500

b
0
0 5 10 15 20 25 30 35
Time (min)
Figure 4. Temperature vs time (a) fire source (b) sample surface (2 cm from the fire)

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 1st Annual Applied Science and Engineering Conference IOP Publishing
IOP Conf. Series: Materials Science and Engineering 180 (2017) 012012 doi:10.1088/1757-899X/180/1/012012

Figure 4 shows that the temperature difference between the fire source and 2.0 cm from the fire spot
is very high. This explains that geopolymer behave as excellent heat isolator and able to protect the
fibers from burning. A research has been conducted to compare heat resistance between calcium silicate
and geopolymer and reported that geopolymers are suitable for fire resistance materials [14]. Figure 5
show the condition of the samples after exposed to fire for 30 minutes. It can be seen that the sample
did not show substantive damage or extensive cracks except on the area of exposed fire. This results
confirmed that the addition of PFL on geopolymers did not change the properties of geopolymer as fire
and heat resistance materials which suitable for high temperature ceramics and composite [15]. The
thermal resistance of the sample was then observed by examining cracks development on the surface of
the materials [16].

Figure 5. The surface of hybrid composite PFL-geopolimer after fire resistance measurement

The acid resistance of the composites was conducted by immersing the samples into 1M H2SO4
solution for 7 days. This measurement was conducted to investigate any damage on the surface of the
samples or fibers due to the intrusion of strong chemical into the bulk of geopolymers. The physical
condition of the samples after removing from the bath is shown figure 6. It can be seen that after 7 days
immersed into strong acid solution, the samples remain strong although their color changed.

a b c d

Figure 6. The samples after 7 days immersing in 1M H2SO4 solution (a) NN 01, (b) NN 02, (c) NN
03, (d) NN 04

It was observed that after 7 days, the pH of the acid solution remain 1 indicating that the sodium
silicate in the network of geopolymer did not leached out and react with H2SO4 solution and hence
increase the pH of the solution. It is worth mentioned that the samples contained higher volume of PFL

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 1st Annual Applied Science and Engineering Conference IOP Publishing
IOP Conf. Series: Materials Science and Engineering 180 (2017) 012012 doi:10.1088/1757-899X/180/1/012012

were the most resistant to acid attack as there were no cracks observed on their surfaces. Extensive crack
was observed on sample NN01 which is pure geopolymer. Altough it is not clear, apparently this result
indicates that the PFL plays important role in preventing physical damage of the composite due to acid
attack. Further study need to be conducted to confirm this finding. This finding is similar to a previous
research on geopolymers concrete immersed in H2SO4 and found that there were no mass loss or physical
damage observed [17, 18, 19].
Figure 7 shows SEM characterization of hybrid composite geopolymers-PFL. Figure 7(a) is the
morphology of geopolymer without pineapple fiber. The surface of geopolymer consists of unfully
reacted fly ash particles and other minerals originated from the raw materials

a b

Figure 7. SEM image of hybrid composite PFL-geopolymer (a) 0% PFL (b) 0.4% PFL (c) 1.2 % PFL

Figure 7 (b) is SEM image of the sample contain 0.4% PFL in which the fibers surrounded by the
matrix of geopolymer and the remaining fly ash particles. The space between fibers maybe as a result
of polishing the sample prior to SEM examination. Figure 7 (c) is the image of the sample which contain
1.2% PFL. It can be seen that the volume of unreacted fly ash particle increase as the volume of fibers
increase. This condition was undesirable since a strong between matrix and aggregate can only be

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 1st Annual Applied Science and Engineering Conference IOP Publishing
IOP Conf. Series: Materials Science and Engineering 180 (2017) 012012 doi:10.1088/1757-899X/180/1/012012

achieved in more homogenous matrix. This is the main reason why the compressive strength of this
sample is much lower than the other samples. Further work is needed to improve the chemical bond
between the matrix and the fibers aggregate.

4. Conclusion
The addition of pineapple fibers into the geopolymers matrix produced a new type of inorganic hybrid
composite. The fibers were found to improve the mechanical properties, compressive and flexural
strength of the composites. The addition of pineapple fibers was also found did not change the nature of
geopolymers as a fire or acid resistance material. Microstructure examinations show that the space
between the geopolymers matrix and pineapple fibers reduce the mechanical strength of the resulting
composite.

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IOP Conf. Series: Materials Science and Engineering 180 (2017) 012012 doi:10.1088/1757-899X/180/1/012012

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