4th International Conference on Process Engineering and Advanced Materials

The Effect of Incineration Temperature to the Chemical and Physical

Properties of Ultrafine Treated Rice Husk Ash (UFTRHA) as
Supplementary Cementing Material (SCM)
Muhd Fadhil Nuruddina, Siti Asmahani Saada,b, Nasir Shafiqa,* and Maisarah Alib
a
Civil and Environmental Engineering Department, Universiti Teknologi PETRONAS, Bandar Seri Iskandar, 32610, Perak, Malaysia
b
Material and Manufacturing Engineering Department, Kulliyyah of Engineering, International Islamic University Malaysia, 53100 , Kuala Lumpur.

Abstract

One of the important criteria of supplementary cementing material (SCM) in concrete is to possess high content of reactive si lica that is
essential in concrete strength development. Indeed, it is proven that rice husk ash (RHA) contains high amount of amorphous silica that is vital
in the reaction of SCM in concrete. However, usage of conventional RHA is unfavourable in current concrete industry. One of the reason that
hindered the utilization of conventional RHA nowadays is due to its properties inconsistency namely chemical and mineralogical properties. This
phenomenon occurs due to sensitivity of the material towards burning temperature. In this regard, improvement on the RHA properties by
introduction of thermochemical pretreatment prior to burning procedure is seen as an excellent way to reach the goal. In this paper, the effect of
burning temperature to the characteristics of pretreated rice husk ash were tested. Raw rice husk was pretreated using 0.1N hydrochloric acid
(HCl) and heated at 80oC. After that, the pretreated rice husk was mechanically activated by high energy planetary ball mill for 15 minutes at
speed of 300rpm and ball-to-powder ratio (BPR) of 15:1. The effect of burning temperature to its chemical composition, particle size analysis,
and microstructure properties of ultrafine treated rice husk ash (UFTRHA) were determined accordingly. As for amorphous silica content of the
optimum sample was recorded as 97.00% incinerated at 700oC with three hours of pretreatment soaking duration. In terms of particle size analysis,
it was also observed that, burning temperature of 700oC, pretreated at three hours were recorded to produce finest size of UFTRHA where d(0.1),
d(0.5) and d(0.9) were obtained as 1.417 µm, 4.493 µm and 14.884 µm respectively.

© 2016 The Authors. Published by Elsevier Ltd.

Peer-review under responsibility of the organizing committee of ICPEAM 2016.

Keywords: Ultrafine treated rice husk ash (UFTRHA) ; Supplementary cementing material (SCM) ; high energy milling.

1. Introduction

Green technology approach is essential in reducing global carbon footprint to mother earth. This phenomenon encourages
explorations of the application of supplementary cementing materials (SCM) in recent concrete industry. SCM are commonly
used in concrete as admixtures to enhance its properties and also to promote greener concrete production. In light of
incorporating SCM into concrete production, rice husk ash (RHA) is regarded as one of them due to high silica content.
Production of RHA is done via thermal activation, which is burning process of the rice husk from agricultural waste.
Rice plant is a type of plant that has the ability to absorb the silica content from soil. The absorbed silica is then eventually
assimilates into its structure during the growth [1]. Therefore, the outer part which refers as rice husk possesses high silica content
with value of more than 80% [2]. Approximately 1000 Million tons of rice is annually produced in the world, which usually leaves
about 400 Million tons of rice husks as a waste material [3]. Hence, the potential of producing ash from husk is about 100 million
tons per annum. Therefore, utilizing RHA in concrete is possible. Furthermore, high content of amorphous silica and high specific
surface area (SSA) of RHA are possible to be achieved by adopting suitable burning condition [4].
A thorough study has been done on addition of conventional RHA in concrete. This is simply due to its content that possesses
high amount of silica content. Nevertheless, quality of rice husk ash produced is still compromised. According to International Rice
Research Institute [5], the rice husk is very sensitive towards incineration or burning process. As the consequences, properties
consistency of conventional RHA produced is compromised. This is the main reason that leads towards unfavorable usage of this
material as SCM in current construction sector [6-7]. Realizing the weakness of the material, some of researchers found that the
impurities can be greatly eliminated through thermochemical pretreatment process using inorganic acid i.e. hydrochloric acid (HCl)
and nitric acid (HNO3) [7-9]. The thermochemical pretreatment process is able to reduce the sensitivity of RHA towards burning
temperature [6]. Therefore, in this paper, the main focus is to identify the effect of various burning temperature to the characteristics
of treated RHA produced accordingly.

© 2016 The Authors. Published by Elsevier Ltd.

Peer-review under responsibility of the organizing committee of ICPEAM 2016.
 Author name / Procedia Engineering 00 (2016) 000–000

2. Methodology

2.1. Ultrafine treated rice husk ash (UFTRHA) pretreatment process

Raw rice husk was obtained from local rice factory (BERNAS) located in Sungai Ranggam, Perak. Prior to incineration
procedure, the rice husk was treated with 0.1N analytical grade (A.G.) hydrochloric acid (HCl). The specimens were soaked and
heated at 80⁰C in the acid solution. After completion of pretreatment process, the samples were washed using distilled water until
it neutral pH obtained and dried using laboratory oven at 110 ⁰C. It was then burned by using conventional furnace in laboratory.
The burning process was done at 700⁰C and 800⁰C with 1 hour retention time. The ultrafine treated rice husk ash (UFTRHA) was
then ground using planetary ball mill for 15 minutes with ball-to-powder ratio (BPR) of 15:1 and rotation speed at 300rpm.

2.2. Characterization of ultrafine treated rice husk ash (UFTRHA)

Effect of incineration temperature to produce ultrafine treated rice husk ash (UFTRHA) were determined via several tests.
Hence, chemical composition of UFTRHA prepared at various burning temperatures were examined using X-ray fluorescence
(XRF) test. The test was done for UFTRHA sample that undergone pretreatment in 0.1N HCl solution at 80oC. The analysis was
done by using spectrometer of Bruker Axs S4 Pioneer. The test was in accordance to BS EN 12677.
On the other hand, particle size analysis was done using Malvern instrument mastersizer, model Scirocco 2000. As for
microstructure analysis, both unground NTRHA and UFTRHA were carried out by using field emission scanning electron
microscopy (FESEM), model Zeiss Supra 55 VP instrument.

3. Results and Discussion

3.1. Chemical composition of UFTRHA

As for chemical composition determination of UFTRHA, X-Ray Fluorescence (XRF) data is summarized in Table 1.

Table 1. Chemical composition of ultrafine treated rice husk ash (UFTRHA) pretreated for 4 hours at various burning temperature.
Chemical Chemical content percentage of UFTRHA using
composition 0.1N HCl with soaking duration at 4 hours (%)
700 oC 800oC
SiO2 97.00 80.10
P2O5 1.63 2.12
Fe2O3 0.25 13.70
CaO 0.46 0.48
Al2O3 0.09 -
K2O 0.11 2.07
Na2O - -
MgO - 0.89
MnO - 0.24
SO3 - -
Cl - -
ZrO3 0.25 0.12

Based on the experimental result, it can be observed that the highest oxide content of the treated rice husk ash is silica (SiO2).
In addition, the SiO2 composition in UFTRHA incinerated at 700oC has highest value among other samples that were prepared at
800oC. According to the XRF analysis result, the SiO2 content in UFTRHA sample produced at 700oC increased with percentage
values of 21.10% as compared to the samples extracted at 800oC. This finding also indicates that the ideal burning temperature to
produce UFTRHA is 700oC.
 Author name / Procedia Engineering 00 (2016) 000–000 3

3.2. Physical properties of UFTRHA

Mechanical milling is one of feasible method to be used in order to reduce size of UFTRHA powder particle. This milling
mechanism is attainable using planetary ball mill. In this regard, several parameters of the mechanical milling process are
considered namely milling speed, ball-to-powder ratio (BPR) and duration of grinding. Table 2 tabulates the particle size analysis
of UFTRHA at different pretreatment duration and various burning temperature with milling speed, BPR and grinding duration of
300rpm, 15:1 and 15 minutes respectively.

Table 2. Particle size analysis of UFTRHA at different burning temperature for 1 to 3 hours of soaking time.
Pretreatment Burning Particle Size (µm)
Grinding parameters Soaking time Temperature
d(0.1) d(0.5) d(0.9)
(hour(s)) (oC)
1 700oC 1.434 4.552 13.996
800oC 1.377 4.798 15.470
BPR: 15:1 2 700oC 1.436 4.508 14.334
Grinding speed: 300rpm
Grinding duration: 15 minutes 800oC 1.181 4.521 17.637
3 700oC 1.417 4.493 14.884
800oC 1.641 4.501 15.331
High speed of the grinding process resulted in greater velocity of the ball movements in the milling bowl. Therefore, shearing
impact between grinding media (balls) and feed stock (UFTRHA) occurs vigorously in the system hence the smaller particle size
obtained. Based on the data in Table 2, UFTRHA that had been treated for three hours and incinerated at 700oC has finest particle
size compared to other UFTRHA samples with d(0.1), d(0.5) and d(0.9) of 1.417µm, 4.493µm and 14.884µm respectively.

3.3. Morphological characterization of UFTRHA

In order to understand the morphological properties of UFTRHA, field emmision scanning electron microscopy (FESEM) images
after three hours of pretreatment soaking duration with pretreatment and incineration temperatures at 80oC and 700oC respectively
were captured. Fig. 1 (a) and 1 (b) display the FESEM images for unground and ground UFTRHA respectively.
Based on investigation of the first FESEM image, it is observed that these particles possesses membranous cavity naturally and
vesicular. On the other hand, vesicular particles in UFTRHA sample that undergone milling process has been broken into small
sections, giving the approximate diameter of the ground particles ranges between 7.259µm to 14.920µm. Form this findings, it can
be deduced that milling process will lead towards reduction of particle size and hence high specific surface area. The effect of
grinding process is illustrated by Van et al. [10] as shown in fig.2.

a b

Fig. 1. (a) FESEM images of unground UFTRHA after three hours of pretreatment soaking duration; (b) ground UFTRHA with pretreatment and incineration
temperatures at 80oC and 700oC respectively.

Fig. 2. Influence of grinding process to mesoporous structure of rice husk ash particle and its particle condition [10].
 Author name / Procedia Engineering 00 (2016) 000–000

4. Conclusion

The results obtained shows that, the correct burning temperature in incineration stage plays an important role in terms of
enhancing the chemical, physical and morphological properties of UFTRHA. This is essential in order to produce high quality
supplementary cementing material (SCM) for concrete technology application. As for the chemical composition analysis, the
highest purity of silica content (SiO2) is achieved by incineration at 700oC of three hours pretreated rice husk. On the other hand,
the highest silica content (SiO2) of the UFTRHA sample was recorded at 97.00% with particle size median of 4.493µm.

Acknowledgements

The author would like express profound gratitude to the Ministry of Education of Malaysia (MoE) for funding the research work
under MyRa Grant Scheme. The author also wishes to thank to the staffs of Department of Civil Engineering and Department of
Chemical Engineering, Universiti Teknologi PETRONAS for their kind assistance in this research.

References

[1] R.G. Smith and G.A. Kamwanja, The use of Rice Husk for making a Cementitious Material, Proc. Joint Symposium on the Use of Vegetable Plants and their
Fibers as Building Material, Baghdad, 1986.
[2] F. Siddique, Waste materials and by-products in concrete: with 174 tables. Springer Press, 2008.
[3] International Rice Research Institute. Rough Rice Production by Country and Geographical Region 1961-2004. Rome: FAOSTAT Database, 2005.
[4] P.K. Mehta, Rice husk ash – a unique supplementary cementing material. In:Advances in concrete technology. 2nd edition. CANMET, pp.41–44, 1994.
[5] International Rice Research, Rough Rice Production by Country and Geographical Region in 1961- 2004, FAOSTAT Database, 2005.
[6] Q. Feng, H. Yamamichi, M. Shoya and S. Sugita, Study on Pozzolanic Properties of Rice Husk Ash by Hydrochloric Acid Pretreatment, Cement and Concrete
Research, 33 (2004) 521-526.
[7] C. Park, A. Salas, C.W. Chung and C.J. Lee, Freeze-thaw Resistance of Concrete using Acid Leached Rice Husk Ash, KSCE, Journal of Civil Engineering,
18 (2014) 1133-1139.
[8] A. Salas, S. Delvasto, R.M. De Gutierrez and D. Lange, Comparison of Two Processes for Treating Rice Husk Ash for Use in High Performance Concrete,
Cement and Concrete Research, 39 (2009) 773-778.
[9] A.G. Vayghan, A.R. Khaloo and F. Rajabipour, The Effects of Hydrochloric Acid Pre-treatment on the Physicochemical Properties and Pozzolanic
Performance of Rice Husk Ash, Cement and Concrete Composites, 39 (2013) 131-140.
[10] V.-T.-A. Van, C. Rößler, D.-D. Bui, and H.-M. Ludwig, Mesoporous Structure and Pozzolanic Reaction of Rice Husk Ash in Cementitious System,
Construction and Building Materials, 43 (2013) 208-216.