Cement & Concrete Composites 55 (2015) 162168

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Cement & Concrete Composites

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

Studies on effects of burning conditions and rice husk ash (RHA)

blending amount on the mechanical behavior of cement
Ru-Shan Bie , Xing-Fei Song, Qian-Qian Liu, Xiao-Yu Ji, Pei Chen
School of Energy Science and Engineering, Harbin Institute of Technology, Harbin 150001, PR China

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

Article history: The properties of RHA samples obtained at different conditions in mufe furnace and their effects on the
Received 20 July 2013 mechanical behavior of cement have been studied. The properties were characterized by SEM, XRF, XRD
Received in revised form 3 September 2014 and specic surface area. The effect of using RHA as a partial replacement for cement has been
Accepted 15 September 2014
investigated by compressive and exural strengths test. It is showed that in mufe furnace 600 C is
Available online 28 September 2014
the appropriate temperature for RHA preparation with large specic surface area due to the existences
of nanoscale and amorphous SiO2. While, long combustion time could increase pozzolanic activity of
Keywords:
RHA. The presence of K could decrease the specic surface area and increase the residual carbon content
Rice husk ash (RHA)
Specic surface area
which content should be control strictly. RHA obtained in proper conditions can be used as cement
Pozzolanic activity additive to increase compressive and exural strengths of cement mortar specimens. It is veried that
Cement RHA replacement ratio of 10% (by weight) has the best enhancement effect on cement strength.
Strength 2014 Elsevier Ltd. All rights reserved.

0. Introduction problem how to utilize rice husk will be solved fundamentally,

Rice husk is an agricultural waste which has a considerable
quantity of over 40-million tons per year in China [1,2]. Rice husk
can be used as boiler fuel to generate electricity or steam. But it also
can contribute about 20% of its weight to RHA after incineration [3].
So RHA is usually treated as industrial waste and hard to be
exploited and utilized [4]. How to deal with rice husk completely
has become an urgent problem. Generally, SiO2 accounts for 15
20% of rice husks mass and a conservative estimate is 1020%
[5]. Exploitation and utilization of the SiO2 in RHA has become a
major research subject in recent years [612]. Ouyang studied
RHA on a nanoscale by using test method such as SEM and EDX.
Analysis showed that amorphous SiO2 in rice husk exists in the
form of nanoparticles and more than 90% (in mass) of the RHA that
obtained in low-temperature of 600 C is made up of amorphous
SiO2. And they has also conrmed that using low-temperature
RHA as additive to replace cement at certain proportion can
improve the strength of the cement [13]. SiO2 of this kind has a
large specic surface area as well as high pozzolanic activity, which
makes it be a kind of high quality mineral cement admixture. Wu
pointed out that RHA is expected to approximate the effect of silica
fume. If RHA can be used as highly active cement additive, the
Corresponding author.
which will turn waste into wealth as well as reduce the cost
of cement industry to realize winwin for economy and environ-
ment. Feng et al.s research substituting RHA for cement to add into
cement indicated that RHA can improve the pore structure, namely
pores become smaller and the number of harmless pores that less
than 20 nm is signicantly increased [14]. The compressive
strength of cement increases as its maximum pore sizes and aver-
age pore size become smaller. Signicant reduction of Ca(OH)2 in
cement and the improvement of its pore structure are the main rea-
sons for the compressive strength increase of RHA cement [15].
Burning condition is one key factor to affect the strengths of
RHA blended cement. Malhotra and Mehta burnt rice husk under
uncontrolled combustion process within the range 600850 C
[16]. Rukzon et al. used the RHA obtained from open burning in
a small heap of 20 kg rice husk with maximum temperature of
self-sustained burning of 650 C at total burning time of 24 h
[17]. Ganesan et al. burned the uncontrolled red husk residue at
650 C and kept constant for a burning time of 1 h [18]. All above
researches get satisfactory results.
Mixture proportion is another key factor to affect the strengths of
RHA blended cement. RHA addition to cement tends to improve its
compressive strength, chloride penetration resistance (mainly
when it replaced 10% of the Portland cement). Ganesan et al. con-
cluded that cement containing 15% of RHA showed an utmost com-
pressive strength and loss at elevated content more than 15% [18].

http://dx.doi.org/10.1016/j.cemconcomp.2014.09.008
0958-9465/ 2014 Elsevier Ltd. All rights reserved.
 R.-S. Bie et al. / Cement & Concrete Composites 55 (2015) 162168 163

Zhang et al. suggested 10% RHA replacement exhibited upper

1.3. Experimental method
strength than control OPC at all ages [19]. Dakroury and Gasser
reported that using 30% RHA as a replacement of part of cement
1.3.1. Rice husk test
could be considered optimum for all content of W/C ratios in inves-
Different section surface properties of the rice husk were inves-
tigated mortars because of its high value of compressive strength
tigated with SEM and EDX. Microstructure and chemical elements
[20].
of rice husk sample with deposited Au lm by ion sputtering were
The objectives of this work are to nd out proper conditions to
examined after vacuum ltration.
produce RHA which could be used as cement additive, which can
also provide experimental data for industrial processes. If cement
can be partially replaced with RHA, it will not only dispose well 1.3.2. Preparation and analysis of RHA
of waste but also reduce the high cost of concrete. RHA samples The rice husk samples were introduced to about 1/3 of the vol-
were obtained at different conditions in mufe furnace. The charac- ume of a 90  60 mm crucible. Thermal treatment of the rice husk
terizations of RHA were investigated by relative instruments. At samples was carried out in a mufe furnace with its door half
last, portland cement was replaced by RHA at various percentages opened to ensure sufcient air in it. The heating temperature
to make mortar samples. The compressive and exural strengths (600 and 700 C) and time (one and two hour) with heating ramp
were tested. of 5 C/min were controlled. In order to ensure its full combustion,
the rice husk needed to be stirred manually once using a dipper of
about 20 cm-long before the thermal treatment. The different sam-
1. Experimental programme
ples were represented with a unique designation throughout this
paper. For example, RHA600-1 h designated the RHA sample pro-
1.1. Materials used
duced at the temperature of 600 C for one hour. RHA600-2 h
and RHA700-1 h had the similar meanings. Chemical composition
1. Rice Husk. Rice husk collected from Harbin, Heilongjiang
of RHA and OPC used in the present investigation is shown in
province was used in the present experimental investiga-
Table 2.
tion. It is tough and rough, with high lignication degree,
high friction and high heating value, as well as good
porousness. Its composition and physical properties are 1.3.3. Preparation and testing of cement specimen with RHA
given in Table 1. Cement mortar specimens were made with the RHA samples
2. Cement. Ordinary portland cement (OPC) 42.5 conforming obtained in different burning conditions, namely RHA600-1 h,
to China standard GB175-200 was used in the present RHA600-2 h and RHA700-1 h, mixed in as additive as per China
experimental investigation. The cement was produced by standard GB/T17671-1999. Grinded RHA substituted for cement
Harbin Yatai cement plant. by quality proportions of 0%, 5%, 10% and 20%, respectively. The
3. Sand. Standard sand produced by Xiamen Aisio was used. prepared cement mortar was cast in 40  40  160 mm steel
mould after being stirred for 20 min and compacted on a table
1.2. Test instruments vibrator for 5 min. After curing for 24 h in a humid environment
of 20 2 C, the specimens were demoulded and placed immedi-
1. Mufe furnace. YX-HF type ash analyzer manufactured by ately in water tank for further curing to prescriptive ages. Strength
the Changsha Youxin industrial co., Ltd. conforming to the tests of each specimen were conducted at various ages. For each
China standard GB/T212-2001 was used, the main body of combination of burning condition and blending amount, three
which is mufe furnace. Oven temperature range is from identical specimens were tested at the ages of 3, 7 and 28 days.
ambient temperature to 1000 C and heating ramp is from The average exural strength of the 3 specimens was reported as
5 to 10 C/min.
2. Specic surface tester. 3H-2000BET-A type automatic Table 2
nitrogen adsorption specic surface tester provided by Chemical composition of RHA and OPC.
Harbin university of science and technology was adopted.
Chemical composition OPC RHA600- RHA600- RHA700-
3. SEM/EDX. HITACHI type scanning electron microscopy (%) 1h 2h 1h
with energy-dispersive X-ray provided by School of materi-
Silicon dioxide (SiO2) 24.07 92.09 93.00 93.42
als and engineering, Harbin institute of technology was Aluminium oxide (Al2O3) 8.75 0.10 0.10 0.12
used to obtain scanning electron micrographs of the RHA Ferric oxide (Fe2O3) 2.51 0.07 0.07 0.07
samples. Calcium oxide (CaO) 53.13 0.97 0.92 0.92
4. XRD. Rigaku D/max-r B type rotatory anode harrow X-ray Magnesium oxide (MgO) 4.49 0.53 0.45 0.37
Sodium oxide (Na2O) 0.21 0.11 0.27
diffractometer was applied to determine the crystal
Potassium oxide (K2O) 4.04 3.62 3.26
structure and average size of RHA. Phosphorous oxide 0.96 0.91 0.68
5. Strength testing machine. YAW-300C type automatic con- (P2O5)
stant stress compression & exure testing machine with an Titanium oxide (TiO2)
accuracy of 1% provided by School of civil engineering, Har- Sulphur trioxide (SO3) 3.25 0.55 0.46 0.44
Loss on ignition 0.64 1.52 1.48 3.24
bin institute of technology was employed in compressive
and exural strength test.

Table 1
Composition and physical of rice husk.

Components (%) Moisture Crude ber Xylogen Pentosan Crude protein Ash Ethyl ether extract
7.516.0 35.545.0 21.022.0 16.022.0 2.53.0 13.022.0 0.71.3
Physical properties Bulk density (kg/m3) Angle of repose () Fuel value (MJ/kg) Heat conductivity (W/(m C))
96160 42 12.616.8 0.0840.209
164 R.-S. Bie et al. / Cement & Concrete Composites 55 (2015) 162168

result of exural strength test. The compressive strength was Table 3

tested after exural strength test. The 6 specimens left were used EDX results of the surfaces.

for compression test and the average compressive strength was Position Si K Ca Fe
reported as the compressive strength of this kind of cement mor- Outer surface 97.4480 2.5520 0 0
tar. Measured strength value whose calculated error exceeded Outside section 88.1826 10.3188 0.9998 0.4988
ten percent (10%) of the average strength value was eliminated Inside section 74.4240 21.5704 2.8320 1.1736
and the average strength was recalculated. So repeated until all Inner surface 93.4450 3.5572 2.5622 0.3188

the errors of values involved in calculation were within 10% of

the average strength, this average strength was reported as the
nal strength of the cement mortar. 2.2. The appearances of RHA

The appearances of RHA obtained at different conditions are

2. Results and discussion
2.1. Microstructure and chemical elements analysis of rice husk
SEM photographs and EDX analysis of outer and inner section
surface of the rice husk are showed in Fig. 1 and Table 3. It can
be seen that the outer surface of rice husk is smooth and its struc-
ture is dense covered with orderly bulges. EDX analysis reveals
that the outer surface is constituted by dense SiO2. Between inner
and outer surfaces there is a loose reticular interlayer, which is
made of criss-cross plate pieces and contains a plenty of pores of
10 lm. Because of its massive existence and large size, the pores
are easy to be found by SEM, which is called reticular honeycomb
structure. The reticular structure is mainly composed of protein,
sugar, lignin, cellulose and some metallic oxide.
The EDX analysis shows that the outer surface and inner sur-
face is mainly constituted by SiO2, with potassium (K) as the main
metal element. The interlayer can be divided into two parts. Out-
side section relies on the longitudinal framework formed by SiO2,
with lattices lled by Ca, Fe and K. In inside section, Si content of
the reticular structure signicantly reduced while all kinds of
metal elements content obviously increased. It indicates that
metal elements, especially K, are mainly involved in the formation
of the reticular structure, which also directly affects the carbon
removal process in rice husk combustion [20]. The degree of car-
bon removal has a direct effect on the specic surface area of RHA
[21]. Therefore, the key technology for the preparation of RHA
with high active and large specic surface area is to guarantee
the structural porosity of SiO2, remove carbon and some metal
impurity.
shown in Fig. 2. RHA obtained at 600 C is slightly grey in color.
And the color of RHA600-2 h is little whiter than RHA600-1 h. It
means the residual carbon content of RHA obtained at 600 C is
low which is shown in Table 2. But there are some black particles
in RHA700-1 h. It means there is more residual carbon in RHA700-
1 h. So the loss on ignition RHA700-1 h is higher which is shown in
Table 2. Temperature has great impact on the residual carbon con-
tent of RHA. If the temperature is raised to the decomposition tem-
perature of K2O, the unburned carbon surface will get entrapped in
the melt. Once carbon is entrapped in the potassium rich melt, it
could not be burned completely as it does not contact with air
directly [22].
2.3. Effects of burning conditions on specic surface of RHA
2.3.1. Specic surface area test and XRD analysis results of RHA
Specic surface area and EDX of RHA samples obtained on dif-
ferent burning conditions are showed in Table 4. XRD analysis
results are showed in Fig. 3.
Table 4 shows that Si contents of all samples were very high
(>89 m2/g), but the specic surface areas have some differences.
The specic surface areas of RHA obtained at 600 C are much
greater than that of 700 C. It also can be seen that specic surface
area has relationship with K content. When K content is around 6%,
specic surface areas are 85.74 and 90.21 m2/g. But when K con-
tent increases to about 8%, the specic surface area decreases to
26.95 m2/g. Fig. 3 shows that SiO2 in 600RHA-1 h and 600RHA-
2 h is amorphous because there are not obvious peaks. But there
were two obvious peaks of 700RHA-1 h. It means that SiO2 in

(a) Outer surface (200) (b) Side section surface (300)

Fig. 1. SEM photographs of the outer and side section surface of rice husk inner surface.
 R.-S. Bie et al. / Cement & Concrete Composites 55 (2015) 162168 165

Fig. 2. The appearances of RHA.

Table 4
Specic surface area and EDX results of different RHA.

RHA samples Specic surface Si (%) K (%) Ca (%) Others (%)

area (m2/g)
RHA600-1 h 85.74 91.5145 6.1247 1.9750 0.3858
RHA600-2 h 90.21 90.9104 6.0948 1.9428 1.0520
RHA700-1 h 26.95 91.1827 8.1360 0.4530 0.2283

(a) SEM of RHA600-1h (b) SEM of RHA700-1h

Fig. 4. SEM of RHA600-1 h and RHA700-1 h.

can be explained by the gazed surface of sheets. But SiO2 in

RHA600-1 h and RHA600-2 h is amorphous. The SiO2 forms discus-
sions are consistent with XRD results (Fig. 3). Another one is
whether there are nanometer scale particles which is called nano-
scale SiO2 particles [13]. The presence of nanometer scale particles
makes the specic surface area very large.

2.3.3. Effects of burning time on specic surface of RHA

Fig. 3. XRD analysis of RHA samples.
700RHA-1 h is crystallized which could be tridymite-O. Tempera-
ture could affect the SiO2 form obviously.
2.3.2. Effects of burning temperature on specic surface of RHA
The results of SEM of RHA samples at small times are showed in
Fig. 4. By the volatile and carbon combustion process stripping, the
internal reticular porous structure with high SiO2 content is expos-
ing. Therefore, the outer surface of rice husk is shed or partially
shed. In order to research the main factors that inuence the spe-
cic surface area of RHA, smaller scale morphologies of different
RHA samples are shown in Fig. 5. Fig. 5 shows that three RHA sam-
ples all have many sheets which are vertical and horizontal inter-
laced. Those sheets constitute a reticular porous structure. It can be
seen that there many small granular particles on the sheet of
RHA600-1 h and RHA600-2 h shown in Fig. 5a and b. The sizes of
particles are very small with nanometer scale (0.1100 nm). How-
ever, there are few granular particles and the surface of sheets in
RHA700-1 h has been glazed.
Table 2 shows that specic surface areas of RHA600-1 h and
RHA600-2 h are similar and very large, and that of RHA700-1 h is
very small. By analyzing Fig. 5, there might be two reasons. The
one is the form of SiO2. SiO2 in RHA700-1 h is crystallized which
Because the RHA obtained at 600 C has a higher activity than
RHA obtained in 700 C, 600 C was chosen as the test temperature.
Fig. 5 clearly shows that the density of the sheets and granular par-
ticles in 1 h-combusted RHA is much smaller than that of 2 h-com-
busted RHA. It comes to a theoretical conclusion based on previous
analysis that it is the number of particles on RHA grid that deter-
mines its specic surface area. As shown in Table 2, the 2 h-com-
busted RHA has a larger specic surface area than 2 h-combusted
RHA. In fact, nitrogen adsorption method measurement showed
that the specic surface area of RHA600-1 h and RHA600-2 h were
85.74 m2/g and 90.2 m2/g, respectively. It illustrates that the
extension of burning time is conducive to increase the density of
the nano-size particles agglomerate and the specic surface area
of RHA, but the effect is not so obvious. The difference of the spe-
cic surface area of RHA600-1 h and RHA600-2 h is quite modest
and both can meet the needs of the cement industry.
2.4. Results of RHA cement strength test and analysis
2.4.1. Effect of RHA blending amount on the mechanical behavior of
cement
The effects of blending amount of different RHA to the strength
of cement are shown from Figs. 68, respectively. Fig. 6a shows
that compressive strengths of four cement replacements by
166 R.-S. Bie et al. / Cement & Concrete Composites 55 (2015) 162168

(a) RHA 600-1h (b) RHA 600-2h (c) RHA 700-1h

Fig. 5. SEM of RHA samples (1000).

(a) Compressive strength (b) Flexural strength

Fig. 6. The effects of blending amount of RHA600-1 h to the strength of cement.

(a) Compressive strength (b) Flexural strength

Fig. 7. The effects of blending amount of RHA600-2 h to the strength of cement.

RHA600-1 h had different behaviors at different curing time. At
3 days, four compressive strengths were similar. During 37 days,
there was a coincidence in the strength development tendency
between 10% and 20% replacements. And the same trend had hap-
pened between 0% and 5% replacements, but both were lower than
the former two. At 28 days, compressive results ranking was
10% > 20% > 5% > 0%. Moreover, compressive results of cement
replacements by RHA600-2 h had the same trend as RHA600-1 h
(Fig. 7a). However, the compressive strength of RHA700-1 h behav-
ior had different from those two RHA (Fig. 8a). At 3 and 7 days, 0%
and 5% results were close and higher than 10% and 20% which com-
pressive strength was the minimum. But at 28 days, compressive
results ranking was 5% > 0% > 10% > 20%. Only 5% results was
greater than 0%, while 10% result was very close to 0%. From the
above results it can be seen that RHA obtained at 600 C had
enhanced effect when blended in cement with three replacements
(5%, 10% and 20%), and 10% replacement effect was the best. But
the replacement effect of RHA obtained at 700 C had different
behaviors. Although 5% and 10% replacement results had not obvi-
ously enhanced effect (10% had reduced effect), those two effects
could be acceptable. But 20% replacement signicantly reduced
compressive strength which could not used as cement additive.
The reason is that RHA produced at 600 C is a kind of highly active
cement additive with high pozzolanic activity due to its
 R.-S. Bie et al. / Cement & Concrete Composites 55 (2015) 162168
(a) Compressive strength
Fig. 8. The effects of blending amount of RHA700-1 h to the strength of cement.
(a) Compressive strength
Fig. 9. The effect of RHA burning conditions to the strength of cement.
amorphous SiO2 (Fig. 3) and high specic surface area (Table 4). So
it can greatly improve the compressive strength when increasing
its blending amount within 10%. However, when the blending
amount exceeds 10%, the compressive strength declined because
the content of cement in the specimen dropped considerably.
While, RHA produced at 700 C has low pozzolanic activities
because of the crystallized SiO2 (Fig. 3) and low specic surface
area of 26.95 m2/g.
As cement additives, each RHA sample had its own different
effect for exural strength. At the age of 28 days, exural results
ranking of RHA600-1 h and RHA600-2 h were 10% > 5% > 20% > 0%
and 0% > 20% > 5% > 0% respectively. For RHA obtained at 600 C,
each replacement could help further enhancement in exural
strength, and 10% replacement enhancement effect was the best.
For cement with RHA700-1 h, exural results ranking was
20% > 10% > 0% > 5%. 10% and 20% replacement could greatly
enhance exural strength which was different from the other two
RHA samples. Only 5% replacement of RHA700-1 h could decrease
exural strength among all replacement results. Compared with
600RHA-1 h and 600RHA-2 h samples, 700RHA-1 h had crystallized
SiO2, more residual carbon (loss on ignition was greater) which
were different from the other two RHA samples. Although there
were not relative references, we think it was the result of the high
hardness SiO2 and high residual carbon content. And further study
should be done to nd out more convincing evidences.
2.4.2. Effect of preparation conditions of RHA on the mechanical
behavior of cement
From the comparison and analysis of effect of RHA blending
amount on cement mechanical behavior, it is easy to gure out
167
(b) Flexural strength
(b) Flexural strength
that 10% blending amount of large specic surface area RHA is
the optimum addition proportion to cement, so the analysis below
is based on 10% blending amount (Fig. 9).
As shown in Fig. 9a, on one hand, the compressive strength of
specimen with RHA600-1 h approximates that of RHA600-2 h
while the compressive strength of specimen with RHA600-2 h is
a little higher than that of RHA600-1 h at 28 days. This illustrates
that burning time has enhancement effect on the compressive
strength of cement specimen but very slight. On the other hand,
the compressive strength of specimen with RHA700-1 h is lower
than that of the original sample in the whole period, which illus-
trates that the specic surface area of RHA has a direct effect on
the compressive strength of corresponding cement specimens.
Fig. 9b shows that the exural strength of specimens with
RHA600-2 h and RHA700-1 h is higher than the original sample,
which illustrates that besides specic surface area, carbon content
and the crystallinity of SiO2 are also the factors that can affect the
exural strength of cement. But considering the errors, experiment
condition and engineering application, exural property is usually
not considered too much when compressive property is requested
strictly.
2.5. Discussions towards industrial processes
From the above results, it can be seen that burning rice husk in
mufe furnace at low temperature (600700 C) can obtain high
activity RHA which could be used as cement additive. It provides
an efcient way to deal with rice husk which is low temperature
combustion. In real industrial applications, circulating uidized
bed (CFB) can realize burning rice husk at low temperature. Based
168 R.-S. Bie et al. / Cement & Concrete Composites 55 (2015) 162168
on engineering experience, a 75 t/h CFB which bed material is
quartz sand solely burns rice husk well when bed temperature is
around 750 C. RHA obtained appear white and the carbon content
of y ash is below 3%, which means the combustion effect is good
enough. Therefore there is not challenge to decrease the burning
temperature in industrial processes due to loss of efciency. Com-
bined this study and real industrial processes, further study can be
carried out to nd out a new technology to utilize rice husk which
might be power-cement additive generation process.
3. Conclusion
1. In mufe furnace, rice husk could burn more completely at
low temperature (about 600 C) than high temperature. At
high temperature, K2O could decompose that causes more
residual carbon in RHA.
2. In mufe furnace, 600 C is the appropriate temperature for
preparation of RHA with large specic surface area due to
the existences of nanoscale and amorphous SiO2. And the
present of K has great impact on specic surface area of
RHA. It could obvious decrease with the K content
increasing.
3. In proper condition, RHA could be used as cement additive
and could enhance cement mortar strength. And 10% RHA
blending amount is the optimum proportion to enhance
cement mortar strength. It provides a feasible way to treat
rice husk which could not only reuse the energy but also
reduce the volume completely.
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