Construction and Building Materials 173 (2018) 10–16

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Construction and Building Materials

journal homepage: www.elsevier.com/locate/conbuildmat

Effects of cellulose, hemicellulose, and lignin on the morphology

and mechanical properties of metakaolin-based geopolymer
Hanzhou Ye a,b, Yang Zhang a,b,⇑, Zhiming Yu a,b, Jun Mu a,b
a
Beijing Key Laboratory of Wood Science and Engineering, Beijing Forestry University, Beijing 100083, China
b
Ministry of Education Key Laboratory of Wooden Material Science and Application, Beijing Forestry University, Beijing 100083, China

h i g h l i g h t s

 Alkaline degradation of hemicellulose was found in FTIR.

 Hemicellulose resulted in insufficient geopolymerization detected in SEM.
 Lignin led to the porous morphology and brittle fracture of geopolymer.
 Cellulose fibres caused the dense structure and ductile failure of geopolymer.
 Good bonding was detected between cellulose fibres and geopolymer matrix.

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

Article history: Natural fiber-reinforced geopolymer has attracted wide attention in construction and building materials
Received 25 December 2017 due to its low cost, low density, and excellent mechanical properties. Cellulose, hemicellulose, and lignin
Received in revised form 24 February 2018 are the three basic components of natural fibres, and were investigated to reveal their influence on the
Accepted 3 April 2018
metakaolin-based geopolymer. Comparative evaluations were investigated via morphology analysis
Available online 6 April 2018
and mechanical strength analysis. The results showed distinct microstructures and mechanical properties
of the geopolymer-based materials with cellulose, hemicellulose, and lignin, respectively. A low content
Keywords:
(5 wt%) of lignin, cellulose, and hemicellulose enhanced the flexural and compressive strength of pure
Geopolymer
Fibres
geopolymer. Higher lignin and hemicellulose led to the porous morphology, lower density, and brittle
Composites fractures of geopolymer-based composites, which reduced the flexural and compressive strength in these
Cellulose geopolymer-based composites. It was noted that the degree of geopolymerization was clearly lowered by
Hemicellulose the alkaline degradation of hemicellulose. With the increase in cellulose content, in contrast, the denser
Lignin structure and fewer pores of the geopolymer matrix were detected, as well as ductile failures of
geopolymer-based composites. Good bonding was also shown between the geopolymer matrix and cel-
lulose fibres without remarkable degradation. The results of this study will facilitate a better understand-
ing of the effect of lignocellulosic biomass in natural fibre-reinforced geopolymers and should serve as
the basis for further research and applications.
Ó 2018 Elsevier Ltd. All rights reserved.

1. Introduction and building materials, and specific industrial applications

Geopolymer, by reduction of CO2 emissions, has emerged as an
environmentally friendly alternative to Portland cement thanks to
its high compressive strength, low shrinkage and creep abilities,
excellent inflammability, and exemplary durability [1–5]. Thus,
geopolymer can be used in a wide range of applications, such as
civil infrastructure (roads and railways), sustainable construction
⇑ Corresponding author at: College of Material Science and Technology, Beijing
Forestry University, Tsinghua East Road 35, Beijing 100083, China.
E-mail address: bjfuzhangyang@bjfu.edu.cn (Y. Zhang).
(radioactive immobilization and contaminant encapsulation)
[6–10]. However, like most ceramics, pure geopolymer suffers from
brittleness problems, which can be overcome with fibre reinforce-
ment in the geopolymer matrix [11,12].
Growing attention to environment and climate change has
piqued people’s interest in natural material production and envi-
ronmental protection materials. It is generally recognized that nat-
ural fibres derived from wood, bamboo, cotton, flax, etc. [12–15]
have been widely applied to reinforce the geopolymer matrix or
to produce lignocellulosic biomass-based materials with geopoly-
mer binders due to these fibres’ advantages with regard to natural

https://doi.org/10.1016/j.conbuildmat.2018.04.028
0950-0618/Ó 2018 Elsevier Ltd. All rights reserved.
 H. Ye et al. / Construction and Building Materials 173 (2018) 10–16 11

abundance, recyclability, low cost, low density, excellent mechan-
ical properties, and nontoxicity [16,17].
Many previous studies dealt with natural fibres as a unit. In fact,
natural fibre, in terms of chemistry, is a biopolymer composite
composed mainly of a network of cellulose (40–60 wt%), hemicel-
luloses (20–40 wt%), and lignin (10–25 wt%) [18,19]. The content of
ambient temperature before curing under different conditions: ambient tempera-
ture for group G, and dried at 80 °C for 48 h for group GH (preheating treatment),
respectively. Specimens were then cured for 7 days at room temperature before
testing. The codes of the specimens are listed in Table 3.
2.4. Characterization

these three chemical components in several natural fibres [20–23]
is listed in Table 1. As shown, cellulose, hemicellulose, and lignin
are the major components of natural fibres (72.3–99.5 wt%), albeit
in quite different lignocellulosic biomass from one species to
another. If the different effects of cellulose, hemicellulose, and lig-
nin on geopolymer can be found, it will be possible to better under-
stand the bonding mechanism between natural fibres and
geopolymer, and to choose which natural fibre is best suited to
the development of natural fibre-reinforced geopolymer
composites.
The objective of this work was to investigate the influence of
the common chemical composition of natural fibres, especially cel-
lulose, hemicellulose, and lignin, on geopolymer properties. Com-
parative evaluations were investigated via morphology analysis
and mechanical strength (flexural and compressive strength) anal-
ysis. The results of this study will facilitate improved understand-
ing of the lignocellulosic biomass in natural fibre-reinforced
geopolymers to serve as the basis for further research and
applications.
2. Materials and methods
2.1. Materials
2.4.1. Fourier transform infrared (FTIR) spectroscopy
The dry samples (10 mg) were dispersed in a matrix of KBr (70 mg), followed by
compression at 12 MPa for 2 min before being tested with a Vertex 70 FTIR spec-
trophotometer (Bruker, Ettlingen, Germany) in the spectral range from 4000 to
400 cm 1.
2.4.2. Scanning electron microscopy (SEM)
The cross-sectional microstructures of the fracture surfaces of the composite
specimens were tested after flexural testing. Micro-images of the geopolymer-
based composites coated with gold were examined via SEM (Quanta FEG 250, FEI,
Eindhoven, Netherlands) at 10 kV.
2.4.3. Mechanical tests
The densities of the specimens were calculated before the mechanical tests, and
the results for each specimen were the average of at least three repeated tests.
Three-point bend tests were used to evaluate the flexural strength (80 mm  20
mm  10 mm) with Instron 3365 Universal Testing Machine (Instron, Norwood,
MA, USA) at a speed of 1 mm/min and a specimen span of 64 mm. All flexural tests
per sample were repeated more than five times, and the average values were
reported. The compressive strength (30 mm  20 mm  10 mm) was determined
using a MMW-50 mechanical testing machine (Jinan Resistance Test Machine Co.,
Ltd., Shandong, China) at an applied speed of 1 mm/min. The average values of com-
pressive strength for each sample were obtained by repeating the test at least three
times.

High purity grade cellulose fibres (medium), hemicellulose (xylan), and lignin
were supplied by Sigma (St Louis, MO, USA). A commercial metakaolin (MK) (Meta-
maxÒ, BASF, Germany) was used as the aluminosilicate source. The chemical com-
positions of MK were measured by X-ray fluorescence (XRF) (XRF-1800, Shimadzu,
Japan), the results of which are presented in Table 2. The particle size distribution
(PSD) of MK (dispersed in water) was assessed with a Mastersizer 2000 particle size
laser analyzer (Malvern Instruments Ltd, Malvern, UK). The values of the PSD of MK,
d10, d50, and d90 were 1.120 lm, 4.120 lm, and 12.966 lm, respectively.
2.2. Activator solution
The activator solution for geopolymerization was made by mixing analytical
grade sodium hydroxide (NaOH) with sodium silicate (Na2SiO3) (Wuxi Yateks Joint
Chemical Industry Co., Ltd., Jiangsu, China). The volume ratio of Na2SiO3/NaOH was
2.5. The molar ratio (SiO2/Na2O) of the activator solution was maintained at a value
of 1.33 using 10 M NaOH.
2.3. Composite preparation
Different contents of cellulose, hemicellulose, and lignin (5 wt%, 10 wt%, or 20
wt%) were mixed with MK. An activator solution was then added to the mixture to
obtain the mortars. The mortars were stirred and cast onto open Teflon molds at an
3. Results and discussion
3.1. FTIR analysis
The FTIR spectra of the geopolymer-based composites are dis-
played in Fig. 1. The wide vibration bands around 3500 cm–1 and
1652 cm–1 exhibited in all spectra were attributed to O–H stretch-
ing and bending, respectively [24–26]. The intensity of the peaks at
451 cm–1 was associated with Si-O-Si bending vibration [27].
Another intense band was centered around 1020 cm–1, corre-
sponding to the Si-O-Al and Si-O-Si vibration bands of the geopoly-
mer. In addition, the chemical composition of natural fibres in all
geopolymer-based composites were represented in the peaks at
2912 cm 1 and 1460 cm 1, corresponding to the alkane CH
stretching vibrations of the methylene groups as well as the CH3
asymmetric deformation vibrations or CH2 scissor vibrations
[28,29]. Notably, the peak around 1610 cm 1 of carboxylate anion
(COO ) was detected in G-H20, indicating ionization of carboxylic
acids due to the alkaline degradation of hemicellulose [30,31].

Table 1
Content of cellulose, hemicellulose, and lignin in several natural fibres.

Natural fibre Cellulose (wt%) Hemicellulose (wt%) Lignin (wt%) Total (wt%)
Cotton 89.7 1.0 2.7 93.4
Flax 80 13 2 95
Hemp 74.1 7.6 2.2 83.9
Sugar cane 51.8 27.6 10.7 90.1
Bamboo 54.6 11.4 21.7 87.7
Coconut 51.3 11.7 30.7 93.7
Wheat straw 38 36 22 96
38.0 29.0 15.0 82
33.2 24.0 15.1 72.3
28.8 39.1 18.6 86.5
Rape straw 36 37 24 97
37.6 31.4 21.3 90.3
Spruce + bark 42 27 26 95
41.0 24.3 30.0 95.3
50.8 21.2 27.5 99.5
Poplar wood 50 30 20 100
12 H. Ye et al. / Construction and Building Materials 173 (2018) 10–16

Table 2
Chemical composition of MK.

Oxide SiO2 Al2O3 TiO2 Fe2O3 Na2O CaO SO3 P2 O5 MgO

MK 54.59 43.03 1.42 0.47 0.24 0.07 0.06 0.06 0.06

Table 3
Nomenclature for the geopolymer and geopolymer-based composites.

Sample Code MK Cellulose Hemicellulose Lignin Activator

(g) (g) (g) (g) (g)
G (or GH)-0 500 – – – 700
G (or GH)-H5 500 – 25 – 700
G (or GH)-H10 500 – 50 – 700
G (or GH)-H20 500 – 100 – 700
G (or GH)-L5 500 – – 25 700
G (or GH)-L10 500 – – 50 700
G (or GH)-L20 500 – – 100 700
G (or GH)-C5 500 25 – – 700
G (or GH)-C10 500 50 – – 700
G (or GH)-C20 500 100 – – 700

3.3. Geopolymerization analysis

The SEM micrographs, on a smaller scale, of the geopolymer

matrix in geopolymer-based composites are shown in Fig. 3. As
reported in previous literature [32,33], the geopolymer matrix of
the composites was found to consist not only of the geopolymer
gel phase but also the partially reacted metakaolin and the plate-
shaped voids left behind from remnant metakaolin. The geopoly-
mer gel was formed through the accumulation of nanoscaled pre-
cipitates (geopolymeric micelles) [34]. These micelles were
connected and formed obvious pores in group G-H and group
GH-H, indicating a lower degree of geopolymerization. In contrast,
the denser structure of the geopolymer matrix was detected in the
other geopolymer-based composites, suggesting higher geopoly-
merization in the geopolymer matrix. This likely occurred because
the alkaline environment for geopolymerization was weakened by
the main degradation products from hemicellulose, carboxylic
acids, in accordance with the FTIR results. The retardation effect
on geopolymer by hemicellulose was also detected during the cur-
ing process through visual inspection. It was noted that the pure
geopolymer and geopolymer-cellulose/lignin composites could
harden within one day, while it took two days or more to form hard
Fig. 1. FTIR spectra of the geopolymer-based composites.
composites of geopolymer-hemicellulose composites.

3.4. Bonding of geopolymer and cellulose fibres

3.2. Morphology analysis
The cross-sectional microstructures of the fracture surfaces of
the specimen are shown in Fig. 2. A dense structure with fewer
pores was detected in the pure geopolymer specimens (Fig. 2A0)
and geopolymer-based composites with low cellulose, hemicellu-
lose, and lignin added (Fig. 2B0, C0, and D0). However, porous mor-
phology, particularly a wide-ranging size distribution of random
pores, was readily apparent in group G-H, group GH-H, group G-
L, and group GH-L with increasing additions of lignin and hemicel-
lulose. These pores were mainly due to water escape in group G-L
during the curing process, while CO2 and water caused by alkaline
degradation of hemicellulose also contributed to the formation of
pores in group G-H. It is interesting that the number of visible
pores was less in the geopolymer-based composites with higher
cellulose fibre content because the pores were filled with fibres.
There was no obvious difference between morphologies of the
geopolymer-based composites with or without preheating before
the curing process.
Whole cellulose fibres can be detected clearly in the geopoly-
mer matrix in the SEM images of G-C20 and GH-C20 (Fig. 4). The
potential bonding mechanism between geopolymer and cellulose
is shown in Fig. 4 E. Clearly, the stinging or sheet-shaped portions
of stripped cellulose were embedded in the geopolymer matrix of
the interface (arrowed in Fig. 4 A through D) after the stretching
process during flexural testing. These results denote good bonding
between the cellulose and the geopolymer matrix without remark-
able cellulose degradation among the highly alkaline geopolymer
conditions. The same phenomenon was also detected in other
fibre-reinforced geopolymer materials [35,36].
3.5. Density
The density of the geopolymer-based composites is shown in
Fig. 5. The increasing contents of hemicellulose and lignin, espe-
cially hemicellulose, exerted a slight negative effect on the density
of geopolymer-based composites due to the obviously porous mor-
phology in the geopolymer-based composites (Fig. 2B1, B2, C1, and
 H. Ye et al. / Construction and Building Materials 173 (2018) 10–16 13

Fig. 2. SEM micrographs of pores in geopolymer-based composites.

Fig. 3. SEM micrographs of the geopolymer matrix in geopolymer-based composites.

C2). The density was nearly unchanged, however, with the increas- density was deemed to be much lower after preheating treatment,
ing content of cellulose. In other words, the effect of content on which concurred with the trend of mechanical strength in the
density was not remarkable in group G-C and GH-C. In addition, geopolymer-based composites.
14 H. Ye et al. / Construction and Building Materials 173 (2018) 10–16

Fig. 4. SEM micrographs of the interface of (A and B) G-C20 and (C and D) GH-C20, and (E) the potential bonding mechanism between geopolymer and cellulose, respectively.

Fig. 6. Flexural strength of the geopolymer-based composites.

Fig. 5. Density of the geopolymer-based composites.

3.6. Flexural strength

The flexural strength of the geopolymer-based composites with

cellulose, hemicellulose, and lignin is shown in Fig. 6. The flexural
strength of pure geopolymer (G-0) was 8.07 ± 1.38 MPa. The max
flexural strength was shown with low additions of cellulose, hemi-
cellulose, and lignin in G-L5, G-C5, and G-H5 as 10.66 ± 0.78 MPa,
9.00 ± 2.00 MPa, and 9.58 ± 1.22 MPa, respectively. In addition, it
can be seen from Fig. 6 that a decreasing trend of flexural strength
was exhibited in the geopolymer-based composites with higher
hemicellulose and lignin, which is different from the cellulose-
reinforced geopolymer composites. The flexural strength reduced
with increasing lignin and hemicellulose content, due to increasing
pores and a low degree of geopolymerization (mainly for group G-
H and group GH-H), which led to the loose geopolymer matrix
structure observed in Fig. 3B1, B2, and BH. According to the litera-
ture, fibres can control the cracking of the matrix by bridging
across the cracks and providing a post-cracking behaviour Fig. 7. Compressive strength of the geopolymer-based composites.
[37,38]. However, the expected excellent flexural strength, com-
pared with group G-L, group G-H, group GH-L, and group GH-H,
was not detected in group G-C and group GH-C. The increasing 3.7. Compressive strength
amount of short cellulose fibres exerted little positive effect on
the flexural strength of composites, even causing a decrease in flex- The effects of cellulose, hemicellulose, and lignin on the com-
ural strength in short natural fibre-reinforced biodegradable resin pressive strength of geopolymer is presented in Fig. 7. As shown,
[39]. the compressive strength of G-0 was 28.84 ± 3.25 MPa. The max
 H. Ye et al. / Construction and Building Materials 173 (2018) 10–16 15

Fig. 8. Failure images of the geopolymer-based composites.

compressive strength of group G-L, group G-C, and group G-H was 4. Conclusions
detected in the 5 wt% cases to be 33.47 ± 5.33 MPa, 36.22 ± 8.31
MPa, and 27.88 ± 8.62 MPa, respectively. Moreover, the compres- In this study, geopolymer-based composites were produced to
sive strength decreased slightly with higher contents of cellulose, investigate the influence of the cellulose, hemicellulose, and lignin
hemicellulose, and lignin compared to the pure geopolymer speci- of natural fibres on the morphology and mechanical strength of
mens due primarily to density reduction in Fig. 5. This trend was metakaolin-based geopolymer. The conclusions can be drawn as
not obvious in group GH due to the almost irrelevant relationship following:
between density and increasing contents of these composites. It
can be seen in Fig. 7 that the compressive strength of the cellulose (1) A low content (5 wt%) of lignin, cellulose, and hemicellulose
fibre-reinforced geopolymer, in group G-C and group CH-C with enhanced the flexural and compressive strength of pure
similar densities, decreased with higher content to 10 wt% and geopolymer.
increased thereafter. The reason seems to be that cellulose fibres (2) Increasing hemicellulose content clearly lowered the degree
were resistant to crack extension (Fig. 2 D2 through DH). of geopolymerization due to the alkaline degradation of
hemicellulose by generating carboxylic acids, which weak-
ened the alkaline environment for geopolymerization.
3.8. Failure properties
(3) Higher lignin and hemicellulose content led to porous mor-
phology, lower density, and brittle fracture of geopolymer-
The failure images (Fig. 8) are also provided to further clarify
based composites, which resulted in the reduced flexural
the relationship between the chemical compositions of natural
and compressive strength.
fibres and compressive strength. The forms of compressive failure
(4) Increasing cellulose fibres content resulted in denser struc-
differed remarkably in group G-0, group G-H, group G-L, and group
ture, fewer pores, almost unchanged density, and noticeable
G-C. Sudden fragmentation was detected in the pure geopolymer
ductile failure of geopolymer-based composites due to
specimens (Fig. 8 A). Breaking or bursting occurred in the compos-
bridging mechanism of the fibres restraining crack
ites loaded with hemicellulose (Fig. 8 B0 through B2) and lignin
propagation.
(Fig. 8 C0 through C2). However, in composites with high cellulose
(5) Good bonding between the cellulose fibre and the geopoly-
content (Fig. 8 D1 through D2), the original shapes were main-
mer matrix was also observed without remarkable degrada-
tained after peak load, presenting ductile failure due to the
tion of cellulose fibres among the highly alkaline
restraints of crack propagation by the bridging mechanism of fibres
geopolymer surrounding conditions.
[40]. The same behaviour was reported for sweet sorghum fibre-
(6) Preheating treatment reduced the density and mechanical
reinforced geopolymer composites [41].
strength of the geopolymer-based composites.
The main focus of this work was on the effect of the three main
constituents of renewable bio-resources, cellulose, hemicellulose,
and lignin, on the geopolymer’s properties by adding different frac-
tions of these constituents to the geopolymer mixtures. In fact, the Conflict of Interest
cellulose, hemicellulose, and lignin of the natural fibres seldom
exist in the form of isolated chemical substances in real applica- There is no conflict of interest.
tions. They are always combined into a whole by interlinkages.
The combined effect of these constituents should be taken into
consideration in future studies. The combined effect could be Acknowledgements
determined by comparing the geopolymer composited with the
original natural fibre, the physical mixture of the biomass’s con- The authors are grateful for the financial support from the
stituents, and the superposition of individual constituents by Fundamental Research Funds for the Central Universities [grant
drawing on the experience of other research fields [42]. numbers 2017ZY28, 2016ZCQ01].
16 H. Ye et al. / Construction and Building Materials 173 (2018) 10–16

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