Nigerian Journal of Tropical Engineering

Vol. 7, No. 2, 2011, PP. 107 -115, ISSN 1595-5397.

IMPROVING SURFACE HARDNESS OF STEEL USING RICE HUSK

WASTE

P. A. Ihom*, G. B. Nyior**, M. U. Suleiman*, and G. Z. Ibrahim*

*
National Metallurgical Development Centre,
PMB 2116 Jos
Plateau State- Nigeria
**
Metallurgical & Materials Engineering Dept.,
Ahmadu Bello University, Zaria-Nigeria
*E-mail: paulihom@yahoo.co.uk

ABSTRACT
The study improving surface hardness of steel using rice husk has been undertaken. Thermal
diffusion penetration method was used to introduce silicon from the waste rice husk into a
hypoeutectoid steel. The steel had 98.1% iron and 0.383% carbon. The ash from rice husks had
91.9% SiO2. The siliconization process was carried out over a temperature range of 700OC to
820OC and a modeled mathematical equation was used to predict hardness values at elevated
temperatures. The result of the hardness test indicated that the hardness increased from 40.0HRC
to 47.7HRC with increase in temperature of siliconization. The modeled mathematical equation
predicted that at a temperature of 1100OC a hardness value of 66.56HRC can be obtained from
the siliconization process. The study has shown that waste rice husks can be used for metal
siliconization thereby turning waste material into a useful one.

1. INTRODUCTION traffic problems. In dry season smoke is

The management of agricultural waste is a
very serious problem in the developing
world. Agricultural solid wastes constitute a
very serious pollution problem, as every
year millions of tons of agricultural wastes
are burnt around the world releasing large
amounts of CO2 into the atmosphere [1,2].
In Nigeria, for example, the agricultural
areas of the North with commercial centers
for processing of groundnuts, rice and maize
have continued to pose serious problems of
contamination to the environment. Heaps of
groundnut shells, rice husks and maize cobs
can be seen taking up vast expanses of land.
These heaps of wastes sometimes spread-out
to cover the roads creating very serious
seen emanating from these waste dumps
continuously while in the rainy season it is
difficult to burn the waste whereby the
waste decompose, producing bad odour and
pollute close by water sources.
Rice husk is the shell of the grain of Oryza
sativa and it is removed during the
processing of the eatable grain which is
within the husk [2]. Rice husk is a good
source of silicon [2]. It contains silicon in a
reasonable quantity. A lot of work has been
done on industrial and municipal waste
however, probably because majority of
agricultural wastes are not hazardous, not
much attention has been given to the
processing of agricultural waste in

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 Improving Surface Hardness of Steel using Rice Husk Waste
developing countries. According to Itoh et al
[3], a large amount of industrial and
municipal waste is discharged from
manufacturing process and public or
household activities. Some of the wastes are
hazardous when they are incorporated in the
human body as stable solids or dissolved
heavy metallic ions. Other wastes impose
much environmental burden on the ecology
and the circulation system of air, water or
soils of the earth. Agricultural wastes fall
into the last category of wastes. Itoh [4] has
explained that the management of bio-waste
in the advanced countries is not much of a
problem. He said that bio-waste (raw refuse)
can be used for methane fermentation,
synthetic gasification, aerobic microbe
decomposition for compost fertilizer,
carbonization for environment cleanup
materials, while methane fermentation and
synthetic gasification is used as biogas and
in fuel cell and power generation [4].
The use of surface treatment to improve
corrosion resistance, wear resistance, heat
resistance, ornamental properties and
functional properties, friction reduction,
hardness improvement etc is now a known
practice [5, 6]. Surface treatments may be
applied at the completion (or finishing) of
mechanical fabrication of components and
are in every sense finishing processes.
Advances in surface finishing technology
have given rise to high performance
machines and automobiles [7]. Silicon-
carbide coating have a micro-hardness of
3000- 3500kg/mm2 [7]. The use of surface
treatment of cutting tools has led to
improved cutting tool performance as well
as prolonged tool life [8, 9].
The objective of this work is to investigate
the efficacy of waste rice husks as a source
for silicon carbide deposition on metal. It is
also to investigate the possibility of
depositing Si-C/SiC on the surface of metal
using thermal diffusion penetration process
108
as against the conventional method of
physical vapour deposition, chemical vapour
deposition, and wet processes for metal
deposition.
2. Experimental Procedure
2.1 Materials
The materials used were plain carbon steel,
sodium hydroxide, rice husks and water.
2.2 Equipment
The equipment used for the work included;
electric furnace, spectro-lab metal analyzer,
x-ray fluorescence, steel boxes, lathe
machine, hack saw, oven, Rockwell
hardness tester, grinding machine, polishing
disk and metallurgical microscope equipped
with camera.
2.3 Methods
The method adopted in the introduction of
the SiC phase to the plain carbon steel using
rice husk was the thermal propelled
diffusion penetration method.
The plain carbon steel rods of 16 mm
diameter were machined to remove oxide
coatings. It was then cut into lengths of 10
mm. All the specimens were washed in a
mild solution of sodium hydroxide to
remove oils and dirt. The specimens were
then dried and ready for use. The chemical
composition of the steel specimens was
determined using a spectro-lab analyzer at
the National Metallurgical Development
Centre (NMDC), Jos. The chemical
composition of the specimen siliconized at
820oC was analyzed for the composition of
silicon.
The chemical analysis of the rice husk used
for the study was determined in a leaching
test; the result was confirmed in NMDC Jos
using x-ray fluorescence spectrometry. Part
of the rice husks was destructively distilled
 P. A. Ihom, G. B. Nyior, M. U. Suleiman, and G. Z. Ibrahim
under air-tight conditions to produce rice
husk ash, during the thermal propelled
diffusion penetration process; this rice husk
occupied the layer next to the samples.
Untreated rice husk was then used to fill the
remaining part of the siliconizing boxes.
The loaded specimens for siliconization
were then charged into the electric furnace.
The specimens were heated to a temperature
regime of 700OC to 820oC, with a 40oC
interval and a consistent holding time of 6
hours throughout the period of the work. At
the end of each temperature regime the box
was removed and the content quenched in
water to maintain the silicon and the carbon
in solid solution.
2.4 Ageing
The quenched specimens were then
transferred to the electric oven which was
set at 150oC and the ageing of the specimens
was done for 3hrs for each set of specimens.
This treatment was carried out with the
possible hope of precipitating SiC on the
surface of the steel.
2.5 Hardness Test
The age hardened specimens were tested for
hardness using Rockwell hardness tester.
The scale C was selected for the test. The
hardness of the control specimen which was
109
the untreated specimen was also measured.
All the readings were confirmed using a
standard hardness block.
2.6 Microstructure Examination
The specimens were prepared using a
grinding machine with 240 - 600 grit. Two
polishing discs were used; one for pre-
polishing using SiC powder paste (6 and 1
microns) and the second disc was used for
the final polishing using alumina powder
paste (0.5 micron). The polished specimens
were etched using nital and examined under
a metallurgical microscope equipped with a
camera. The microstructure was
photographed using the camera.
2.7 Statistical Analysis and Modelling
The relationship between the hardness
(degree of siliconization) of the
hypoeutectoid steel and the siliconization
temperature was determined using product
moment coefficient of correlation (r) [10]
using equation 1.
r = nΣXY – ΣxΣY/ √nΣx2 – (Σx)2 x √ nΣY2
– (ΣY)2 (1)
Where x is the temperature (T) and Y is the
hardness (H), n is the number of
experiments. The hardness is in HRC and
the temperature is in degree Celsius (OC).
 Improving Surface Hardness of Steel using Rice Husk Waste

Table 1 : Calculation of the Product Moment Coefficient of Correlation (r )

X Y X2 Y2 XY
(Temperature) (Hardness)
700 40.0 490000 1600 28000
740 42.3 547600 1789.29 31302
780 45.8 608400 2097.64 35724
820 47.7 672400 2275.29 39114

ΣX=3040 ΣY=175.8 ΣX2 =2318400 ΣY2 ΣXY

=7762.22 =134140
r= nΣxy- ΣxΣy/ √nΣx2 – (Σx)2 X √nΣy2 – (Σy)2 = + 0.99.
Based on data in Table 1 the following The modeled equation is as in equation 5
simple linear equations were used to model
a mathematical equation for the prediction H=-6.59+0.0665T (5)
of the hardness (degree of siliconzation) at
3. Results And Discussion
elevated temperatures.
3.1 Results
Y=a+bx (2)
The result of the chemical composition of
a=ΣY/n-bΣx/n (3)
the rice husks ash is shown in Table 2. Table
b=nΣXY–ΣXΣY/nΣx –(Σx) 2 2
(4) 3 shows the hardness test result and Table 4
shows the chemical analysis of the hypo-
where, ‘a’ and ‘b’ are constants representing eutectoid steel used for the work. Figures 1-
the intercept and slope. 5 show the microstructure of the siliconized
plain steel.

Table 2: Chemical Composition of Rice Table 3: Hardness Values of the Siliconized

and Unsiliconized Plain Carbon Steel using
Husk Ash Rice Husk at various Temperatures.
Composition % Content
Moisture content 1.30
Protein 0.43 Temperature (oC) Hardness (HRC)
Ash content 1.50 Control sample 39.1
Silica (SiO2) 91.90 (unsiliconized) 40.0
Calcium oxide 0.35 700 42.3
(CaO) 740 45.8
Ferric oxide (FeO) 0.19 780 47.7
Magnesia (MgO) 0.45 820
Alumina (Al2O3) 3.00
Others -

110
 P. A. Ihom, G. B. Nyior, M. U. Suleiman, and G. Z. Ibrahim

Table4: Chemical Composition of as-received Hypo-eutectoid Steel used

Element C Si Mn P S Cr Ni Mo Al Cu Co Ti Nb
% Content 0.383 0.196 0.74 0.066 0.032 0.082 0.038 0.0059 0.010 0.258 0.0055 0.0020 <0.003
Element V W Pb B Sn Zn As Bi Ca Ce Zr La Fe
% Content 0.002 0.020 0.0055 0.0009 0.015 0.0049 0.0058 <0.002 0.0059 0.0041 0.0024 0.0037 98.1

Table 5: Hardness Values of the Empirically Determined and the Hardness Values using the
Mathematical Modeled Equation.

Temperature Empirical Hardness Values Hardness (modeled

o
C (HRC) equation) HRC
700 40.0 39.96
740 42.3 42.62
780 45.8 45.28
820 47.7 47.94

Fig.1: Untreated Specimen with Ferrite Matrix and Uniform Fig. 2: Specimen Siliconized at 700oC, showing a thin dense
Distribution of pearlite X100. Diffusion Layer and a much Lighter Core X100.

Fig. 3: Specimen Siliconized at 740OCShowing Fig. 4: Specimen Siliconized at 780OC Showing a Much Thicker
a thin Dense Diffusion Layer and a lighter Core and Denser Diffusion Layer and a Lighter Core X 100.
X100.

Fig. 5: Specimen Siliconized at 820oC Showing a Large and Dense Diffusion

Layer with a Lighter Core, the Precipitates are Coarse x100.

111
 Improving Surface Hardness of Steel using Rice Husk Waste
3.2 Discussion
3.2.1 Chemical Analysis of the Rice
Husks and the Hypoeutectoid Steel used.
Table 2 shows the chemical analysis of the
rice husk ash used for the siliconization
process, the silicon in the rice husk was
converted to silicon dioxide during the
ashing process. The result showed the
silicon dioxide (SiO2) composition of the
leached ash to be 91.9%. This was
confirmed using x-ray fluorescence
spectrometry; this is a clear indication that
the rice husk is a rich source of silicon.
Other researchers have equally confirmed
the richness of this waste in silicon [11, 12].
Table 4, shows the chemical composition of
the hypoeutectoid steel that was used for the
work. The result showed that the
hypoeutectoid steel has a carbon content of
0.383% and iron content of 98.1%. The
composition of the hypoeutectoid steel
indicates that the microstructure will consist
of pearlite within a ferrite matrix with a
much higher percentage of the later [13, 14].
This type of structure exhibits poor hardness
and low wear resistance. The introduction of
Silicon will increase the silicon content of
the steel which is 0.196% in the surface of
the steel leading to increase hardness and
wear resistance [5]. This was observed in
one of the specimens siliconized at 820oC,
which showed an increase in silicon
composition to 1.124%. The tendency for
the precipitation of SiC phase on ageing of
the steel will also increase leading to
increase hardness and wear resistance.
3.2.2 Hardness Test
Table 3 shows the hardness values of the
siliconized and the unsiliconized
hypoeutectoid steel used. The control
sample which is the unsiliconized steel has a
hardness value of 39.1 HRC. The table
showed that the hardness value increased as
112
the siliconizing temperature was increased
from 700 to 820OC. This agrees with
observations made by Oki [5]. This process
is obviously a temperature dependent
process. According to Oki [5], siliconization
of steel using thermal diffusion penetration
method requires heating for several days;
however, he stated that the time could be
reduced by the use of elevated temperature.
The process is a diffusion controlled process
and so it depends on temperature and time,
because the silicon atoms have to move
through interatomic spaces of the iron atoms
to occupy interstitial positions. This is made
easier at elevated temperature where the iron
has gamma (γ) phase and FCC cubic
structure [15, 16 ]. The degree of
siliconization, therefore depends on the
temperature and the holding or resident time
of the material at that temperature and obeys
this diffusion equation:
D = D0 exp (- ED/ RT)
(6)
Diffusion in a solid is a thermally activated
process, where D is the diffusion, D0 is the
diffusion coefficient, T is the absolute
temperature in kelvin, ED is the activation
energy required to move an atom, and R is
gas constant [16].
For the silica formed during the process to
dissociate, elevated temperature is required
[5]. The degree of siliconization is indicated
by the hardness of the material. The higher
the degree of siliconization the harder and
the thicker the silicon diffusion layer [5].
The relationship between the hardness
(degree of siliconization) of the
hypoeutectoid steel and the siliconization
temperature was determined using product
moment coefficient of correlation (r) using
equation 1.
The product moment coefficient of
correlation (r) is + 0.99. This is a further
 P. A. Ihom, G. B. Nyior, M. U. Suleiman, and G. Z. Ibrahim
confirmation that there is a strong
correlation between the hardness values of
the material and the siliconization
temperature. The temperature is the
independent variable and the hardness is the
dependent variable [10].
According to Oki [5] siliconization takes
time, but to speed up the process, elevated
temperature is required.
The degree of siliconization is reflected in
the hardness of the hypoeutectoid steel. The
degree of siliconization is also higher at
higher temperature [5, 10]. Using equation
5, we can predict the degree of siliconization
at 900oC, 950oC and 1100 oC, as 53.26HRC,
56.59HRC, and 66.56HRC, respectively.
This is because hardness values determined
using the modeled equation give very close
figures to those of the hardness values
determined empirically. For example at a
temperature of 740oC the empirical hardness
value is 42.3 HRC, while the calculated
value using equation 6 is 42.62 HRC.
This result agrees with literatures reviewed
that the degree of siliconization is higher at
elevated temperatures where formed silica
can dissociate into nascent silicon [5, 7].
3.2.3 Microstructure Examination
The microstructure examination covered the
untreated specimen and the siliconized
specimens as represented by Figures 1-5.
The untreated specimen which is a rolled
stock has a sparsely distributed pearlite
structure within a ferrite matrix. Because of
the low magnification of 100 the grain
boundaries are not clear, but the dendrites of
cementite can be clearly seen in the
microstructure. The hardness of this
untreated specimen which is 39.1 HRC
agrees with the structure which is more of an
113
equilibrium structure and is not saturated
with carbon [12, 17]. Figures 2-5 show a
diffusion layer with possible small
precipitates of SiC. The dense area is the
diffusion layer whereas the lighter area is
the substrate. The micrographs were taken at
the interface of the case area and the
substrate; this explains the dark and lighter
areas seen in the microstructure. The
diffusion area increases with the temperature
and holding time but in this case the holding
time was constant. The microstructure is the
confirmation of the hardness and the
siliconization process. A higher resolution
microscope is however required to clearly
see the phases present in the case area.
Further work to study the diffusion layer
using scanning electron microscope (SEM)
and x-ray diffractions (XRD) is ongoing by
the authors. For now based on the hardness
values and the microstructures the authors
can only say that there are precipitates in the
case area nothing can be said about the
composition of the precipitates or of the
presence of silicon and carbon in the
diffusion area. The essence of the research
work has however been achieved, which is
to increase the surface hardness and wear
resistance of the hypoeutectoid steel using
waste rice husks. Some researchers have
however said that higher temperatures and
longer holding time will yield bigger
diffusion layer in the surface of the
hypoeutectoid steel [5, 18]. The aging period
leads to the precipitation of SiC in the
diffusion layer [16].
4. Conclusions
The study, rice husk waste utilization for
improving surface hardness of steel has been
carried out and the following conclusions
have been drawn from the research:
 Improving Surface Hardness of Steel using Rice Husk Waste
1 Rice husk waste is a source of silicon,
which can be utilized in the siliconization of
steel.
2. The hardness of the steel increased as the
siliconizing temperature was increased.
3. The study showed that there is a strong
product moment coefficient of correlation
(r) of +0.99 between the hardness and
siliconization temperature.
4. The relationship between hardness and
siliconization temperature was modeled and
the modeled equation was used to prove that
the degree of siliconization is better at
elevated temperature as this is reflected in
the improved hardness values at elevated
temperatures. The hardness value of
66.56HRC was predicted at a temperature of
1100oC all conditions been equal.
5. The microscopic examination of the
treated steel also revealed a diffusion layer,
thick and denser indicating the presence of
precipitates and solid solution of silicon and
carbon in iron.
5. Acknowledgement
The authors are grateful to the youth
corpers serving with the National
Metallurgical Development Centre, Jos who
assisted in the preparation of the specimens
for test and to staff of the machine shop who
assisted with the cutting of the specimens.
We appreciate you all.
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