Beruflich Dokumente
Kultur Dokumente
Faculty of Materials Science and Chemistry, China University of Geosciences, Wuhan 430074, China
Engineering Research Center of Nano-Geomaterials of Ministry of Education, China University of Geosciences, Wuhan 430074, China
c
Zhejiang Research Institute, China University of Geosciences, Hangzhou 311305, China
b
h i g h l i g h t s
A geopolymer is proposed based on fly ash blended with sawdust.
Relationships between flow, setting time, density and sawdust content are observed.
Sawdust is beneficial for the resistance to cracking and drying shrinkage.
Sawdust exhibits positive effect on compressive and flexural strength after 28 days.
Sawdust addition leads to the formation of an optimal microstructure.
a r t i c l e
i n f o
Article history:
Received 5 October 2015
Received in revised form 5 January 2016
Accepted 17 February 2016
Available online 21 March 2016
Keywords:
Geopolymer
Fly ash
Sawdust
Strength
Pore structure
a b s t r a c t
This work aims to verify the feasibility of utilizing sawdust in geopolymer to make reinforced composites
and broaden application of sawdust in geopolymer. Fresh properties including workability and setting
time, density, nailing ability, drying shrinkage, mechanical strength and microstructure of fly ash
geopolymer activated by sodium silicate and sodium hydroxide solutions blended with 020% of sawdust
by mass with an interval of 5% were investigated.
The experimental results uncover that sawdust addition influences the workability of geopolymer. The
sawdust content is inversely proportional to the setting time and a good linear relation is found between
density and sawdust content. Sawdust is beneficial for the resistance to cracking and drying shrinkage
especially the later ages. Sawdust exhibits little effect on compressive strength before 14 days of curing
and it possesses positive effect after 28 days. 5% of sawdust addition exhibits little effect on flexural
strength regardless of days of curing. The flexural strength increases with increasing content of sawdust.
With the increasing addition levels of sawdust, the porosity decreases and compact matrix can be
observed. Sawdust addition leads to the formation of an optimal microstructure. The results from
mechanical properties and microstructure observation are compatible.
2016 Elsevier Ltd. All rights reserved.
1. Introduction
Relatively low flexural strength and poor resistance to crack
opening and propagation are the main disadvantages of conventional cement concrete [1,2]. Generally, replacement of ordinary
Portland cement (OPC) by mineral admixtures in concrete can
decrease porosity, especially in the long-term [1]. On the other
hand, mineral admixtures such as silica fume can also increase
materials producing high strength and good durability while maintaining an acceptable level of energy consumption for production.
The aforementioned issues about the drawbacks of cement
prompt various researches in an attempt to develop a new cementless binder, and geopolymer is such an emerging alternative binder, which was first developed by Davidovits [5]. Geopolymers
are three-dimensional aluminum silicate inorganic polymers composed by [AlO4] and [SiO4] tetrahedra that are mainly prepared
from aluminum silicates or industrial waste [6] such as fly ash
[7,8], slag [911], metakaolin [12,13] etc. and mixed with an alkali
silicate solution under highly alkaline conditions.
Geopolymer represents an alternative to Portland cement due
to similar or even better binding properties [14,15]. In recent years,
geopolymer has attracted considerable attention due to its early
compressive strength, low permeability, good chemical resistance
and excellent fire resistance behaviour [1622].
Although different source materials can be used to prepare
geopolymer binders, fly ash, represents industrial waste that can
be found all over the world, it is particularly attractive for the synthesis of geopolymers. Fly ash is a by-product of thermal power
plant that produces electricity, it contains an ample quantity of
amorphous alumina and silica. Therefore, it is a suitable and a good
source material for producing geopolymeric binder owing to its
chemical compositions.
The properties of fly ash-based geopolymer concrete have been
studied in the last decades [2328]. Fly ash-based geopolymer concrete has properties favourable for its potential use as a cementitious material due to excellent durability aspects. Some authors
[2932] have reported similar engineering properties of geopolymer concrete that were favourable for its use as a construction
material.
Despite the fact that research in this area is intense and there
are a large number of publications that suggest a wide range of
applications of these materials, FA-based geopolymers are still far
from practical applications on a large scale and many problems
are still need to be further investigated [33].
Traditionally, several methods have been used to strengthen
cementitious materials. The most commonly used method was to
add fibers to reinforce cementitious materials [34]. Fibers are
incorporated into concrete to overcome this weakness, producing
materials with increased flexural strength, ductility, toughness
and improved durability properties [3537]. Adding fibers into
plain concrete has been proved to be an effective method to eliminate its inherent brittleness. The fibers bridge the cracks in the
matrix and transfer the applied load to the matrix, thus fiber reinforced concrete has better post-crack behavior than plain concrete
[38]. The presence of fibers also leads to higher impact resistance
and greater flexural and tensile strengths [39]. These property
enhancements depend on a number of factors including matrix
strength, fiber volume and fiber surface bonding characteristics
[40,41].
However, high cost and health hazard of fibers preparation hinder its application. As one of lignocellulosic biomasses, sawdust is
the by-product from the mechanical milling or processing of timber (wood) into various useable sizes. The production of this waste
is up to 24.15 million m3 per year [42]. The sawdust mainly consists of lignin, cellulose, and hemicellulose. Large amounts of these
wastes were either burnt or land filled. These approaches cause
various environmental problems like air pollution, emission of
greenhouse gases, and occupation of useful land. Therefore, the
disposal of sawdust is getting more and more attentions in recent
years. The abundance and availability of sawdust together with its
relatively low cost guarantee its continued utilization.
Among these disposals of sawdust, mineral-bonded sawdust
composites which combine sawdust with Portland cement [43],
magnesite cement [44] and gypsum [45] have long history, and
601
the earliest commercial mineral-bonded (cement) sawdust composite dates back to 1930 s [46].
As mentioned above, sawdust is either disposed of burning or
land filling. But in recent days, land filling is becoming limited
due to scarcity of waste land and increasing environmental concerns, furthermore, burning also leads to environmental contamination. In this regard, many researches and studies are being
carried out to use sawdust, especially in construction materials
to develop a sustainable way of its disposal. The increasing demand
of cement leads to higher rate of environmental degradation and
more exploitation of natural resources for raw material. The use
of sawdust as partial cement replacement in concrete can reduce
the requirement of cement to a large extent [47].
Researchers [4749] had conducted tests which showed
promising results for sawdust being suitably used to replace
cement partially in concrete. Chowdhury et al. [50] evaluated the
suitability of burnt sawdust as partial cement replacement in conventional concrete. It was concluded that the strength properties of
concrete mixture decreased marginally with an increase in burnt
sawdust contents, but strength increased at later ages. Elinwa
et al. [51] assessed the properties of fresh self-compacting concrete
containing sawdust, they found that the compressive strength
development showed a tremendous improvement over the control.
Aigbomian et al. [52,53] developed a new wood-crete building
material using sawdust. It was able to withstand considerable
amount of impact load and the most suitable for wall paneling or
other non- and semi-structural application with good thermal
insulating properties. Sales et al. [54,55] evaluated the potential
application of lightweight concrete produced with lightweight
coarse aggregate made of the water treatment sludge and sawdust,
by determining the thermal properties, mechanical properties and
possible environmental impact of future residue of this concrete.
Also, Zhou and Li [56] made light-weight wood-magnesium oxychloride cement composite building products with sawdust as
aggregate by extrusion. They reported that the composite exhibited less die swell and better performance in resisting high
temperature.
However, after reviewing the previously published findings, the
effects of sawdust on geopolymer are even not well known, little
information is available about microstructure changes of geopolymer and fly ash was not mentioned. Information of effects of sawdust addition on fly ash geopolymer still requires further
investigation.
Therefore, this present study is devoted to determine the fresh
properties, density, nailing ability, drying shrinkage, mechanical
strength, microstructure evolution and pore structure of geopolymer prepared using fly ash as resource material and activated by
liquid alkaline activator when fly ash was partially replaced by
sawdust at levels ranging from 0% to 20% with an interval of 5%,
by weight.
2. Experimental
2.1. Materials
Fly ash utilized in this study was provided by Shenhua Junggar Energy Corporation in Junggar, Inner Mongolia, China. The micrographs of fly ash were shown in
Fig. 1. Sawdust, which was obtained from a wood workshop as residuals when cutting natural wood, was used as reinforcement component for geopolymer. There
were some wood fibers in the sawdust as observed from naked eyes. The sawdust
with density of 0.79 g/cm3 was incorporated into the geopolymer composites without any special pretreatment. This wood, which is used in both the civil construction and furniture sectors, is highly water absorbent with the water absorption of
67% after immersed in water for 24 h and very light with a regular fiber length
due to its anatomical structure as shown in Fig. 2.
The chemical analysis of starting material mentioned above was listed in
Table 1, the properties of sawdust was given in Table 2.
602
10 m
5 m
2 m
1 m
1cm
10 m
(a)
(b)
Fig. 2. The morphology of sawdust: (a) macro morphology; (b) observed by scanning electronic microscopy.
Table 1
Chemical compositions of fly ash by XRF analysis (mass, %).
Fly ash
a
SiO2
Al2O3
Fe2O3
MgO
CaO
Na2O
K2O
MnO
TiO2
LOIa
29.47
51.72
2.25
0.15
5.21
0.05
0.35
0.03
1.83
8.58
Table 2
The chemical composition of sawdust (mass, %).
Cellulose
Hemicelluloses
Lignin
Extractives
35.9
27.1
32.8
4.2
activated samples during thermal curing and is an important step because water
is necessary for polymerization. After 24 h, all the specimens were released from
the molds and were subjected to further curing in a standard condition of
20 2 C and 90 5% relative humidity up to acquired days for density, shrinkage,
mechanical properties test and microstructure analysis. Setting time test and workability for fresh geopolymer were also carried out.
Sample characterization was conducted on geopolymer paste specimens to
evaluate the effects of sawdust addition on properties of them.
100
90
D90
Cumulative (%)
80
70
60
50
D50
40
30
20
D10
10
0
0.1
10
603
100
Table 3
Particle diameter of fly ash (lm).
Characteristic diameter
Fly ash
Dave
D90
D50
D10
5.33
16.11
5.20
1.03
Fig. 3 shows the particle size distribution of fly ash sample. The characteristic
particle diameters D10, D50 and D90 have been tabulated in Table 3. A wide variation
in particle size was observed in fly ash, of which 90% are less than 17 lm.
Alkali activator applied in this work was a combination of sodium silicate solution and sodium hydroxide (99.2% NaOH) in analytical reagent degree (the mass
ratio of sodium silicate solution to sodium hydroxide equals to 8:1). The liquid portions in the mixture were 10 M sodium hydroxide (NaOH) and sodium silicate (Na2SiO3) with 14.51% Na2O, 33.39% SiO2, and 48.53% H2O. The alkali activator solution
was premixed and left to rest for 24 h at ambient temperature prior to casting. It is
remarkable that liquid activator are prepared by mixing of the sodium hydroxide
solution and sodium silicate at the room temperature, and it liberates large amount
of heat so it is recommended to leave it for about 24 h before use.
Table 4
Mix proportion design for geopolymer paste (mass, %).
Mixtures
Fly ash
Sawdust
SD0
SD5
SD10
SD15
SD20
0
5
10
15
20
100
95
90
85
80
0
5
10
15
20
604
155
SD0
150
700
SD5
650
SD10
Diameter (mm)
145
140
135
SD15
130
125
120
SD20
115
y = -8.6x + 610
R = 0.9747
SD0
600
SD5
SD10
550
SD15
500
450
SD20
400
110
0
10
15
20
10
15
20
14
pH
13
12
11
0
10
15
20
SD5
Density (kg/m3)
SD0
2000
1900
SD10
1800
SD15
1700
y = -25.7x + 2097.8
R = 0.9922
1600
SD20
1500
1400
0
10
15
20
605
606
14
1310
SD0
1510
SD5
1110
SD10
910
SD15
SD20
710
510
310
110
1
14
28
90
SD0
12
SD5
10
SD10
SD15
SD20
6
4
2
0
1
80
SD0
SD5
60
SD10
50
SD15
SD20
40
30
20
10
14
28
90
0.06
Reference
SD5
SD10
14
28
90
70
SD15
SD20
0.05
0.04
0.03
0.02
0.01
reference specimen SD0 at 1, 3, 7 and 14 days. Sawdust exhibits little effect on compressive strength before 14 days of curing. A pronounced increasing in compressive strength can be found at longer
ages after 28 days especially when more than 10% of sawdust is
added, and the increasing is even as high as about 9.6% at 28 days
and 12.1% at 90 days for SD20 compared to SD0, respectively.
Importantly, the changes in compressive strength are modest
with increasing curing ages. Strength at 90 days is nearly the same
with that at 28 days. It can be concluded that early strength of
geopolymer increases rapidly and this is consistent with previously
reported findings [7173]. Yadollahi [71] found that compressive
Fig. 12. The flexural strength of geopolymer with different content of sawdust.
strength increased slowly after 28 days of curing. Ranjbar [72] concluded that geopolymerization was almost complete after 7 days
and the strength gain beyond this period was found insignificant.
Islam [73] also found that most of the specimen achieved 86% of
the 28-day strength at the age of 3-day. Similarly the 7-day and
14-day strengths were 90% and 94%, respectively of the 28-day
strength.
In geopolymer, aluminosilicate gel is the major binding phase
that provides interparticle bonding, which in turn enhances the
macroscopic strength [7476] and takes over the strength gain
behavior of geopolymer paste. Sawdust possesses positive effect
on compressive strength of geopolymer especially at longer curing
ages.
Aigbomian [52] also reported that the compressive strength
increased with increasing content of sawdust. It reflects the compaction of sawdust: relatively small particles and wood fibers at
this point may have filled many gaps between and within them
each other, thus enhancing stress transfer between both materials.
Fly ash particles are generally one to tens of microns in diameter with average particle size of 5.33 lm (see Fig. 3 and Table 3).
Those fine particle materials contribute to the compaction of the
geopolymer matrix (see Figs. 13 and 14).
The alkaline reactivity of fly ash samples was determined
according to Chapelle test described in [77], 1 g of fly ash was mixed
with 1 g of Ca(OH)2 and 100 ml of boiled water. The suspension was
boiled for 16 h and the free Ca(OH)2 was determined by means of
sucrose extraction and titration with a HCl solution. The pozzolanic
activity was 57.5% for fly ash. Higher alkaline reactivity of fly ash
also leads to higher strength after partial replacement.
Based on the analysis mentioned above including fineness and
reactivity, geopolymer with higher strength was obtained. This is
consistent with the findings obtained by Elinwa et al. [51], who
assessed the properties of fresh self-compacting concrete containing sawdust and found that the compressive strength development
showed a tremendous improvement over the control.
To uncover the effect of sawdust addition, specific compressive
strength results are obtained in Fig. 11. Pronounced increase of the
specific compressive strength of geopolymer can be clearly
observed. Partial replacement of fly ash by 5%, 10%, 15% and 20%
of sawdust increases the compressive strength over the reference
sample. Sawdust addition makes it possible to develop lightweight
materials with high compressive strength.
3.7. Flexural strength
Investigation of the ability to resist deformation under load was
done through the flexural test. Flexural strength tests of fly ash
607
0.09
(a)
0.08
0.07
SD0
0.06
SD5
SD10
0.05
SD15
0.04
SD20
0.03
0.02
0.01
0.00
1
10
100
1000
10000
100000
1000000
(a) SD0
(b)
SD0
0.06
dV/dlogD (mL/g)
SD5
0.05
SD10
SD15
0.04
SD20
0.03
0.02
0.01
0
1
10
100
1000
10000
100000
1000000
(b) SD10
(c) SD20
Fig. 13. The morphological changes of geopolymer with different content of
sawdust.
from around 2.2 MPa at 1 day to more than 8.4 MPa at 90 days. In
terms of sawdust reinforced geopolymer, 5% of sawdust addition
exhibits little effect on flexural strength regardless of days of curing.
However, the flexural strength increases with increasing content of
sawdust.
It can be seen that geopolymer with 20% sawdust content
reveals the highest flexural strength for all the specimens regardless of curing ages. Evidently SD20 with highest flexural strength
leads to the conclusion that sawdust possesses positive effect on
reinforcement of flexural strength of geopolymer especially after
28 days of curing and hence the produced geopolymer becomes
denser, stronger with greater durability also indicated by nailing
ability as shown in Fig. 8.
Geopolymer with addition of sawdust possesses higher flexural
strength than reference specimen SD0, which may be ascribed to
that there are more wood fibers in sawdust added specimen which
strengthen the bonding with the geopolymer matrix. Nazari [78]
reported that the highest flexural strength of unreinforced
specimens was 9.5 0.4 MPa and reinforcing of this mixture by
5 wt.% of steel fibres resulted in the highest flexural strength,
11.8 0.9 MPa and concluded that in reinforced specimens, there
is a good adhesion between fibres and geopolymeric paste.
3.8. Microstructure
SEM analyses were carried out on geopolymer specimens
prepared from fly ash comprising sawdust in order to identify
and verify the internal microstructure. It also characterizes the
bonding between sawdust and geopolymer matrix. The bonding
is primarily important to produce a strong geopolymer and serves
as the proof of sawdust reinforced geopolymer composites.
608
Acknowledgments
This work was supported by the National Natural Science
Foundation of China (51502272), the Fundamental Research Funds
for the Central Universities (G1323511543), China University of
Geosciences, Wuhan, China Postdoctoral Science Foundation
(1231512).
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