J. Am. Ceram. Soc.
, 1–5 (2016)
Journal
Potassium-Based Geopolymer Composites Reinforced with Chopped
Bamboo Fibers
Kaushik Sankar,‡ Ruy A. S

a Ribeiro,‡,§ Marilene G. S
a Ribeiro,§ and Waltraud M. Kriven‡,†,**
‡
Department of Materials Science and Engineering, University of Illinois at Urbana-Champaign, Urbana, Illinois 61801
§
Structural Engineering Laboratory, National Institute for Amazonian Research, Manaus, AM 69067-375, Brazil
Bamboo is a fast-growing, readily available natural material
with tensile specific strength equivalent to that of steel (250–
625 MPa/g/cm3). In the pursuit of sustainable construction
materials, a composite was made with potassium polysialate
siloxo geopolymer as the matrix and randomly oriented
chopped bamboo fibers (Guadua angustifolia) from the Amazon
region as the reinforcement. Four-point flexural strength test-
ing of the geopolymer composite reinforced with bamboo fibers
was carried out according to ASTM standard C78/C78M-10e1.
Potassium-based metakaolin geopolymer reinforced with 5
wt% (8 vol%) untreated bamboo fibers yielded 7.5 MPa four-
point flexural strength. Scanning electron microscopy and opti-
cal microscopy were used to investigate the microstructure. In
addition, X-ray diffraction was used to confirm the formation
of geopolymer.
Keywords: geopolymers; composites; kaolinite; fibers; potas-
sium
I. Introduction
1 from around 100°C and the geopolymer undergoes phase
P OLYSIALATE geopolymers are amorphous inorganic poly-
mers that cure at ambient temperatures. Their chemical
structure is made up of cross-linked silica (SiO4) and alumina
(AlO4
) tetrahedral units forming a three-dimensional amor-
phous network with alkali metal cations for charge balance.
Geopolymers are formed by mixing an amorphous alumi-
nosilicate source (like metakaolin which is used in this study)
with a caustic alkali silicate solution. The chemical reaction
proceeds as dissolution of the aluminosilicate source into the
caustic alkali silicate solution, polycondensation of AlO4

and SiO4 tetrahedra into random networks, and precipitation
into circular polysialates.2 Geopolymers are nanoporous and
water is mechanically entrapped in the nanopores.2 Micro-
chemical analysis by TEM and EDS by Kriven et al.3,4
revealed that a fully reacted geopolymer is of the composi-
tion M2OAl2O34SiO211H2O (where M = Na, K or Cs)
when the particle size of metakaolin is 1.2 lm. Duxson
et al.5,6 carried out extensive research on the relationships
between composition, processing, microstructure, and the
properties of metakaolin-based geopolymers (MKGPs) and
found that the best compressive strength is obtained when
the Si:Al molar ratio is 2:1 in geopolymers.
When compared to ordinary portland cement (OPC),
geopolymers have faster setting time and lower density. The
mechanical properties of geopolymers are superior to
P. Colombo—contributing editor
Manuscript No. 38414. Received April 2, 2016; approved August 16, 2016.
Presented in part at the 40th International Conference & Exposition on Advanced
Ceramics and Composites, January 28, 2016 (ICACC-FS1).
**Fellow, The American Ceramic Society.
†
Author to whom correspondence should be addressed. e-mail: kriven@illinois.edu
1
DOI: 10.1111/jace.14542
© 2016 The American Ceramic Society
portland cement in general, but are influenced by the con-
tents of the liquid phase in the mixture, the curing tempera-
ture, and the final porosity of the body.5 The energy required
to produce geopolymer is considerably lower than that
required for OPC. The extent of reduction in energy depends
upon the raw materials used to make the geopolymer.7 They
are processed as a liquid enabling them to be cast into any
shape and cured at ambient or slightly elevated temperatures.
However, like ceramics, pure geopolymers are brittle and
are weak in tension. Their failure is catastrophic with very
little warning signal. On the other hand, they can function as
a matrix to a wide variety of reinforcements to produce a
composite material that improves the ductility of the material
and provides “graceful” failure with sufficient warning
because of various toughening mechanisms.8–13 In addition,
the tensile and flexure strengths are also increased due to effi-
cient load transfer from the matrix to the reinforcement
phase.
Pure metakaolin-based potassium geopolymers (MKGP)
remain amorphous up to 1000°C. The water starts to boil off
transformation into leucite, kalsilite, and remnant glassy
phase starting from 1000°C.14
Geopolymers can be tailored to be a high-strength, envi-
ronmentally friendly, structural material that can be made
using local resources.15 In addition to the mineral reserves
containing aluminosilicates, there are many industrial pro-
cesses that generate slag, fly ash, and other byproducts as
sources of aluminosilicates, so that the raw material for
exploitation of this technology is abundant. Moreover, the
introduction of fibers, particles, and strips of native or natu-
ral materials grown in the Amazon (such as bamboo) in the
production of geopolymeric composites, promote higher
strength, rigidity, and workability, generating green, high-
performance materials. The use of regional and local materi-
als in the production of geopolymeric composites reduce
environmental impacts and raise their practicality in different
situations.
Plant biocomposites (natural fiber reinforcements), have
low density, low cost, and low energy consumption, as well
as neutralizing CO2 production. One such natural fiber rein-
forcement is bamboo. Characteristics of bamboo fibers
include: low-cost,16,17 high tensile strength (200–503 MPa),16–20
low density (0.8–1.4 g/cm3)16–19 and biodegradability;17,19,21,22
absorption of CO2 and production of O2 by three times
more than other plants.17,19 In the pursuit of tough or
semiductile and high strength, green geopolymer composites,
several researchers used natural fibers, such as basalt,8,23,24
corn husk,25 wool,26 jute,11 rice stem,15 fique (or sisal),27 for
reinforcement of MKGP. Adding 10 wt% of 13 lm diame-
ter by 6.35 mm long basalt fibers to potassium-MKGP
yielded 19.5 MPa three-point flexure strength.24 Increasing
the chopped basalt fiber lengths to 12.7 mm yielded a
27.1 MPa three-point flexure strength.23 Sodium-based
geopolymer reinforced with corn husk fiber bundles resulted
2 Journal of the American Ceramic Society—Sankar et al.
in 14.1 MPa four-point flexure strength.25 Sodium-based
geopolymer reinforced with 5 wt% wool fiber bundles
yielded 8.1–9.1 MPa three-point flexure strength.26 Sodium-
based geopolymer reinforced with 30 wt% untreated jute
weave resulted in 20.5 MPa four-point flexure strength.11
Potassium-based geopolymer reinforced with 6.4 wt% rice
stem yielded 18.4 MPa three-point flexure strength.15 Potas-
sium-based geopolymer reinforced with 30 wt% alkali-trea-
ted fique fibers yielded 11.4 MPa four-point flexure
strength.27 Up to this date, we found no published work on
MKGP reinforced with bamboo fibers.
This research investigates the use of bamboo as a struc-
tural reinforcement for geopolymer composites. The bam-
boo-reinforced geopolymer composites (GPCBs) are intended
to replace conventional cements and concretes, using low car-
bon emission and producing sustainable green materials.
II. Experimental Procedures
(1) Bamboo Fibers Processing
The Amazonian tropical bamboo species Guadua angustifolia
was selected based on abundance, accessibility, mechanical
properties, durability, and commercial size criteria. Four-
year-old Guadua culms were collected from a research planta-
tion area,28,29 at the National Institute for Amazonian
Research (INPA) in Manaus, Brazil, and immersed in water
for 3 days for better machine workability. The green bamboo
culms [Fig. 1(a)] were chopped through a chipper (PHT
140 9 400, Pullman Maschinenfabrik GmbH and Co. KG,
Zweibr€ ucken, Germany) and the chips were transformed into
fiber bundles through a Hammer Mill (PZ8, Pullman,
Zweibr€ ucken, Germany) at INPA’s Particleboard Laboratory.
The bamboo fiber bundles (BFs) [Fig. 1(b)] were air-dried,
and filtered by an Allgaier sifter machine through a mesh #4
(12.51–40 mm). Bamboo’s main chemical constituents are
60% cellulose 32% lignin and hemicellulose.30 Minor con-
stituents that account for the remaining 8% are resins, tan-
nins, waxes, and inorganic salts. At the Geopolymer
Laboratory of the University of Illinois at Urbana-Cham-
paign (UIUC), the BFs were washed with deionized water
and set to dry-in two layers of paper towels before utilization.
(a)
(b)
Fig. 1. (a) Water-treated bamboo culms; (b) mechanically attained
air-dried fiber bundles.
(2) Geopolymer Composite Processing
Potassium silicate solution of composition K2O2SiO211H2O
(or potassium “water glass”) was made by mixing fumed sil-
ica (Cab–O–Sil EH-5 Cabot Corp, Tuscola, IL) with KOH
pellets (Fisher Scientific Waltham, MA) dissolved in deion-
ized water according to the reaction:
2KOH þ 10H2 O þ 2SiO2 ! K2 O  2SiO2  11H2 O (1)
Polysialate siloxo-type potassium geopolymer was pre-
pared at the Geopolymer Laboratory by mixing potassium
water glass and Metamax metakaolin (Al2O32SiO2) (BASF
Corp., Florham Park, NJ) (particle size 1.2 lm) mixed in a
high shear mixer (IKA mixer Model RW20DZM, IKA Ger-
many) for 5 min at 1100 rpm to obtain good mixing of the
components. This slurry was then put in a Thinky ARE-250
planetary conditioning mixer (Intertronics, Kidlington,
Oxfordshire, England) that further mixed and degassed the
slurry for fine removal of bubbles. The geopolymerization
reaction can be summed up as follows:
K2 O  2SiO2  11H2 O þ 2SiO2  Al2 O3
(2)
! K2 O  Al2 O3  4SiO2  11H2 O
Chopped bamboo fibers (BF) 5 wt% (~8 vol%) was
slowly added to the geopolymer slurry and manually mixed
until complete integration occurred. The geopolymer com-
posite slurry was poured on to a (110 mm 9 10 mm 9
10 mm) high-strength DelrinÒ mold attached to a vibration
table (FMC Syntron vibrating table, FMC Technologies,
Houston, TX) for more uniform distribution of BFs and less
void formation. The filled mold was held together by clamps,
closed with a DelrinÒ (FMC Technologies) plate and
wrapped in plastic food service film to prevent water loss
during setting and curing. It was then cured for 24 h at 50°C
in a Lab Companion oven (Jeio Tech, Seoul, Korea). Then,
the GPCB samples were demolded and set to dry in a sealed
plastic zip lock bag at room temperature.
After 1 week of drying, the samples were cut to (55 mm 9
10 mm 9 10 mm) using a Drill MasterÒ 4″ tile saw machine
(Harbor Freight Tools Co., Camarillo, CA) with a high-speed
diamond blade for four-point flexure testing. The samples were
tested on the seventh day after curing. Previous studies showed
that metakaolin-based pure geopolymer (MKGP) lost its weight
over time upon exposure to air and was fully dried to reach its
steady-state weight after 7 days.31
(3) Four-Point Bend Testing
Thirty (55 mm 9 10 mm 9 10 mm) GPCB specimens were
subjected to four-point flexure testing (third-point loading
configuration), on the seventh day curing age, according to
ASTM standard C78/C78M-10.32 The average density of
GPCB was 1.57 g/cm3. Tests were carried out by an Instron
testing machine at the Advanced Mechanical Testing and
Evaluation Laboratory (AMTEL) of UIUC. Tests were con-
ducted in stress-controlled mode at a stress rate of 1 MPa/
min as prescribed by the standard. The data acquisition rate
was 20 Hz.
Weibull functions were calculated using a linear regression
method. A distribution function, F, was estimated based on
the flexure strength of 30 samples using the median rank
method shown in Eq. (3) below
i
0:3
Fffi (3)
n þ 0:4
where the flexure strength for each sample is given a rank i
from 1 to n, which is the number of samples in the batch.
The Weibull distribution function is written as shown in
 Geopolymer-Bamboo Composites 3

Eq. (4) below where m is the non-dimensional volume, r is

the stress, ro is the scale parameter, and m is the shape
parameter or Weibull modulus
h i

vðrr Þm
F¼1
e 0
(4)

Since the gage length was the same in all samples, v = 1.

In order to determine the Weibull parameters, Eq. (4) can be
rearranged to obtain Eq. (5) below
  
1
ln ln ¼ m lnðrÞ
m lnðr0 Þ (5)
1
F

This
 1 is of the slope-intercept form of a straight line, so
ln ln 1
F is then plotted versus ln(r), using the approxima-
tion of F given in Eq. (3), and a linear fit is applied for each
data series. The slope of the fitted line then corresponds to
the Weibull modulus, m, and the y-intercept corresponds to
–m ln(ro) which can be solved for the scale parameter, ro.33
The average value rf can be calculated according to the
Eq. (6), where Γ is the Gamma function.
sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
 ffi
Fig. 2. Typical stress–strain curve for GPCB tested in third-point
1 loading.
rf ¼ r0 C 1 þ (6)
m

bamboo fibers improves the average flexure strength by 67%

The standard deviation, S, was calculated using Eq. (7) when compared to pure (0 wt% BF) K-MKGP.8 This pre-
sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
     ffi
liminary strength result of GPCB was lower than some pub-
2 1 2 lished work on geopolymer reinforced with other natural
S ¼ r0 C 1 þ
C 1þ (7) fibers.11,15,23–25 However, this GPCB has a flexural strength
m m
of 7.5 MPa that makes it suitable for several structural appli-
cations given the fact that it can be produced using locally
available reinforcements. A typical stress–strain curve is
shown in Fig. 2. Large strain was observed in all samples
(4) Characterization before the initial vertical crack at the central point. Central
Fractography of post-fractured samples and the interface displacement continued until the fibers stretched to breaking,
between the bamboo fiber and the geopolymer matrix were accompanied by some fiber pullout. This behavior was also
qualitatively analyzed by scanning electron microscopy reflected in the shape of the stress–strain curve (Fig. 2),
(SEM) (JSM-6060LV JEOL USA, Inc., Peabody, MA). Opti- which demonstrated a very smooth behavior without sharp
cal microscopy (Leica Microsystems GmbH, model MZ6, kinks. Therefore, the addition of chopped bamboo fibers
Wetzlar, Germany) was used for fractography on cross sec- provided “graceful” failure with sufficient warning signal for
tions of post-tested flexure samples. the composite.
Phase characterization of pure K-geopolymer was per- The SEM [Fig. 3(a)] image shows an imprint of the fiber
formed by X-ray diffraction (XRD) (Siemens/Bruker D-5000 on the matrix which indicated good contact of the matrix
Model with a copper K-alpha radiation wavelength of with the fiber. The image also shows rough straight line fea-
0.15418 nm). XRD was carried out according to the follow- tures on the matrix which indicates that there was mechani-
ing parameters: scan speed 1°/min with 0.05° increments and cal interlocking and friction between the fiber and the matrix
the scan type was locked in a coupled configuration. when the fiber was pulled out. A cross section of GPCB sam-
ple after flexure testing [Fig. 3(c)] showed fiber pull-out
which is a toughening mechanism. Cracks on the geopolymer
III. Results and Discussion
matrix deflected around the fibers instead of ripping apart
Fiber mass fraction of 5 wt% (volume fraction of 8 vol%) the fiber, thereby, toughening the composite as illustrated in
was chosen for the composite because of processing con- Fig. 3(b), when compared to pure K-geopolymer [Fig. 3(d)].
straints. A fiber mass fraction higher than 5 wt% (8 vol%) This mode of crack deflection at the fiber–matrix interface is
resulted in a composite that was too viscous to be poured characteristic of a weak interface. The weak fiber–matrix
into a mold even with vibration assistance. Pure (0 wt%/vol interface is expected because geopolymers do not bond well
% BF) K-MKGP was already tested by Ribero and Kriven.8 with organics. These toughening mechanisms are responsible
From Table I, it can be inferred that the addition of chopped for the change from sudden failure in the case of pure potas-
sium MKGP to a “graceful” failure with sufficient warning
in the case of GPCB. Figure 3(e) shows the cross section of
Table I. Four-Point Bend Test Results for Pure post-tested flexure sample. Figure 4 illustrates the morphol-
K-Geopolymer36 and GPCB ogy of as-received bamboo fibers. They consist of a large
amount of starch in the parenchymal cells of the fibers
Weibull Scale St. (Fig 4).
avg. (rf) parameter (ro) Deviation 95% C.I.
X-ray diffractogram of the geopolymer matrix is presented
Sample (MPa) (MPa) Shape (MPa) (MPa)
in Fig. 5 where the XRD pattern indicated that the geopoly-
Pure K-GP36 4.5 5.1 2.7 1.8 — mer was X-ray amorphous with an amorphous hump at 28°
GPCB 7.5 8.4 2.9 2.8 6.5, 8.5 two theta. This confirms geopolymer formation without any
crystalline components at room temperature.
4 Journal of the American Ceramic Society—Sankar et al.

(a) (b) (c)

(d) (e)

Fig. 3. (a) SEM micrographs of GPCB tested specimen, showing the impression of the bamboo fiber in the geopolymer matrix; (b) SEM image
of a cross section of a post-tested flexure sample revealing crack deflection around the bamboo-geopolymer interface; (c) Optical microscope
image of a post-tested flexure sample showing fiber pull-out; (d) SEM image of a cross section of a pure potassium geopolymer where there is no
resistance to cracks; (e) SEM image of cross section of a post-tested flexure sample.

Fig. 4. SEM micrograph of untreated Guadua bamboo fibers, Fig. 5. X-ray diffraction pattern of geopolymer matrix confirming
revealing starch (small-round particles) in the parenchymal cells. its amorphous nature.

IV. Conclusions
a sustainable structural material with good flexural strength.
In this study, potassium geopolymer reinforced with ran- The average value of the four-point flexural strength (rf) for
domly aligned, as-received chopped bamboo fibers provided the GPCB tested specimens was 7.46  0.99 MPa. The
 Geopolymer-Bamboo Composites
errors in flexural strengths were calculated based on the 95%
confidence interval (95% CI). SEM micrographs revealed a
weak interface between the bamboo fibers and the geopoly-
mer matrix. The addition of bamboo fibers to geopolymer
not only increased the flexural strength and strain but also
toughened the composite. The failure mode shifted from
catastrophic failure in the case of pure potassium geopolymer
to a more graceful failure in the case of GPCB.
Acknowledgments
This work was partially supported by the U.S Air Force Office of Scientific
Research (AFOSR), through the Tyndall Air Force Base, Florida, under grant
no. FA 9550-06-1-0221. The work of Ruy A. S
a Ribeiro was supported by
CNPq – Conselho Nacional de Desenvolvimento Cient
ıfico e Tecnol
ogico -
Brazil. SEM and XRD were carried out at the Frederick Seitz Materials
Research Laboratory Central Facilities (FS-MRL). Flexural strength tests were
carried out at the Advanced Mechanical Testing and Evaluation Laboratory
(AMTEL) of UIUC. Bamboo collection, fiber preparation, and conditioning
were done at the Structural Engineering Laboratory (LTEE-INPA) and at the
Particleboard Laboratory (LA-INPA).
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