Kufa Journal of Engineering

Vol. 10, No. 1, January 2019, P.P. 29-43

Received 29 November 2017, accepted 14 February 2018

OPTIMIZATION OF STEEL HARDNESS USING

NANOFLUIDS QUENCHANTS
Abbas K. Hussein1, Laith K. Abbas2, Wisam N. Hassan3
1 Department
of Materials Engineering, University of Technology, Iraq. Email:
abbas2000x@[Link]
2 Department of Materials Engineering, University of Technology, Iraq. Email:
3 Kut Technical Institute, Middle Technical University, Iraq

[Link]

ABSTRACT
The goal of this study is to specify the optimal factors for the hardening process (tempering
temperature, the percentage of nanoparticles, type of base media, nanoparticles type and
tempering time) in order to maximize the hardness of medium carbon steel by using Taguchi
technique. An (L18) orthogonal array was chosen for the design of the experiment. The optimum
process parameters were determined by using signal-to-noise ratio(larger is better) criterion.
The important levels of process parameters on hardness were obtained by using analysis of
variance which applied with the help of (Minitab17) software to investigate the effect of
parameters on the hardness. Percentage of volumetric fractions of nanoparticles with three
different levels (0.01, 0.03 and 0.08%) was prepared by dispersing nanoparticles that are (α-
Al2O3, TiO2 and Cuo) with base fluids (De-ionized water, salt solution, and engine oil).
Medium carbon steel specimens were suffered to hardening and tempering heat treatment
process. Tempering temperature was (400℃, 550℃) for (30,45and 60 minutes). Results ended
up with a conclusion that tempering temperature (400℃) had the major influence on hardness
behavior then type of nanoparticles (TiO2) followed by time tempering (30min) then base media
(salt solution) and finally volume fraction of nanoparticles (0.03%).

KEYWORDS: Nanofluids, quenching, hardness, Taguchi technique.

30 Abbas K. Hussein et al.

1. INTRODUCTION
Heat transfer is the driving event on the quenching process, where the specimen is heated to a
required temperature and then immersed into the quenching medium. The hot metal immersed
to be cooled with different stages. Due to high temperatures, a stable vapor film is formed
around the surface of the component. In this stage, heat transfer is very slow because the vapour
film acts as an insulator and occurs by radiation through the vapour phase. Then the surface
temperature of the metal starts to reduce; simultaneously the vapour film starts to collapse. Now
nucleate boiling starts due to the contact of the quenching medium with the metal surface. This
effect is characterized by violent bubble formation as the heat is rapidly removed from the metal
due to the maximum heat transfer. Here the quenching medium plays an important role to
conduct the heat (Baskaran et al., 2016). One of the technical challenges of quenching as a heat
treatment process is to select a quenchant medium that could minimize or eliminate these side
effects while at the same time provide an interface for heat to be transfer from the work piece
to the medium in order to produce the desired properties (Chaves, 2001; Herring, 2010). This
study employs nanofluids as quenchants. Nanofluids is the result of dispersion of nanosized
materials such as nanoparticles, nanofibers, nanotubes, nanowires, nanorods, nanobubbles or
nanosheets in the base fluid like water, oil, acetone, heat transfer fluids, polymer solutions, bio-
fluids and etc. Scientist Choi of Argonne Laboratory (USA) successfully prepared nanofluid in
(1995) (Mukherjee and Paria, 2013). Nanoparticles are in dimension range of (1-100 nm).
Nanoparticles show many different properties than parent material due to increase in surface
area to volume ratio (1000 times larger than microparticles).So, nanofluids enhance many
thermo-physical properties such as thermal conductivity (Taylor et al., 2013). There are
numerous researches on the superior heat transfer properties of nanofluids, especially on the
thermal conductivity. (Hwang et al., 2006; Yu et al., 2009; Mintsa et al., 2009) observed an
important improvement of the nanofluids’ thermal conductivity compared to conventional
coolants. (Park et al., 2004) experimented with copper spheres quenched in nanofluids with
alumina nanoparticles at (5–20 %vol.) and sub-cooling at(293–353 oC). Through this
experiment, the nanofluids have a low boiling rate as compared with pure water. Furthermore,
their investigation showed that the film boiling stage was by-passed to rapid cooling on
successive quenching with unwashed spheres. The researchers have concluded that the stable
vapour film was prevented due to nanoparticle deposition on the sphere surface. The present
study aims to get an optimized effect of quenching media parameters (concentration of
nanofluids, type of the nanofluids, tempering temperature, tempering time and type of the base
media) on the hardness of medium carbon steel to obtain a maximum of the hardness.
 Kufa Journal of Engineering, Vol. 10, No. 1, January 2019 31

2. EXPERIMENTAL PROCEDURE

2.1. Materials
The following materials were used in the nanofluids synthesis:

Nano titanium dioxide (TiO2) powder, nano aluminum oxide(α-Al2O3) powder and copper
oxide (CuO) nanoparticle (supplied by Zhengzhou Dongyao nano materials [Link].). The
properties of these nanoparticles are given on Table 1. Those materials were added to base
media (Deionized water, Salt solution (NaCl+water) and Engine oil). Sodium lauryl sulfate as
a surfactant was used.

Table 1. Physical properties of nanoparticles.

Average Specific bulk True

Nanoparticle Purity Crystal
Particle Size surface area density density Color
material (%) form
(nm) (m2/g) (g/cm3) (g/cm3)
α-Al2O3 50 >99.99 160.1 0.916 3.91 white
TiO2 20 >99.9 220 0.25 3.9 Cube white
CuO 50 >99.9 120 0.30-0.45 6.40 Sphere black

2.2. Nanofluid Preparation

In this research, eighteen types of nanofluid are prepared[(Al2O3/ Deionized water), (Al2O3/ salt
solution), (Al2O3/ engine oil)], [(TiO2/ De ionized water),(TiO2/ salt solution), (TiO2/ engine
oil)], [(Cuo / De ionized water), (Cuo / salt solution), (Cuo / engine oil)] with volume fractions
of (0.01, 0.03 and 0.08%).In this paper, nanofluid was prepared by two step method where the
given nanoparticle is mixed to the base fluid to obtain a suspension. The quantity of
nanoparticles required for preparation of nanofluids is calculated using the law of mixture
formula. The mass of nanoparticles (Mnp) and base fluid (Mnf) are measured with the balance
of (0.0001 g) an accuracy. The weight percentage (ϕ) can be calculated by using Eq (1).

M
np /ρnp
ϕ = Mnp M 1
+ bf
ρnp Mbf

Where:
Φ: volume fraction.
Mnp: mass of nanoparticle (g).
ρnp: density of the nanoparticle(g/L).
Mbf: mass of the base fluid (g).
32 Abbas K. Hussein et al.

ρbf: density of the base fluid(g/L).( Hussein et al., 2013)[10]

A mechanical stirrer was used to achieve a homogeneously dispersed solution, as shown in Fig.
(1-C). This method was based on (Han and Rhi, 2011; Mahendran et al., 2012) [11] [12]. After
preparing the proper mix of the nanoparticles and fluids by a mechanical stirrer, nanoparticles
are dispersed in fluids using magnetic stirrer Fig. (1-A). During the process, Sodium Dodecyl
Sulphate (SDS) surfactant is added to the solution in proper proportions to ensure the stability
of nanofluid. For various purposes, sound energy is used to agitate the particles in a nanofluid.
This process is known as sonication. By breaking intermolecular interaction, sonication is also
used for speed up the dissolution. Sonication is more useful when the magnetic stirring was not
much effective for a given sample. For nanoparticles which were not evenly dispersing in
liquids, sonication is most preferable. The sonication process is achieved in two steps were:

A- Initially Sonicate the mixture continuously for (30 min) with sonicator to obtain a uniform
dispersion of nanoparticles in fluids, this process is achieved with an ultrasonic mixer (LUC –
410(50 Hz,400W)) that shown in Fig. (1-B).

B-Sonicate the mixture continuously for (90 min) with probe sonicator that shown in Fig. (1-
D).

Fig. 1. A-Magnetic stirrer, B- Ultrasonic or bath sonicator C-Electrical blender, D-Ultra

sonicator probe sonicator.
 Kufa Journal of Engineering, Vol. 10, No. 1, January 2019 33

2.3. The material of the research specimens

In this research, medium carbon steel has been used as research specimens. The chemical
composition analysis of the specimens was carried out at the (Specialized Institute for
Inspection and Engineering Qualifying) by x-ray fluorescent. The chemical composition of the
carbon steel is given in Table 2.

Table 2. The chemical composition of medium carbon steel specimens.

Element C% Si% Mn% P% S% Cr% Mo% Ni% Al% Cu% Fe%

Composition % 0.583 1.76 0.790 0.0197 0.0035 0.0351 0.002 0.0135 0.0264 0.033 Bat

2.4. Specimen preparations

First of all, for the experiment, is the specimen preparation. The fifty-four steel samples were
machined by using (CNC) machine to standard dimensions according to (ASTM E8), then the
specimens were grinded and polished.

2.5. Heat Treatment process

Eighteen types of heat treatments were performed, these were quenched and tempered
according to the Table 3. Quenching experiment was performed to harden the medium carbon
steel. The process involved putting the red hot iron directly into a liquid medium. Firstly, all
specimens were heated-up to an austenitizing temperature in an electric furnace (carbolite cwf
1200 muffle furnace). The specimens were held at (900°C) for sufficient time (approximately
an hour) to ensure uniformity of temperature throughout the entire volume to achieve a
homogeneous structure of austenite. This was followed by the quenching treatment where each
group of samples was quenched in different quenching mediums (nanofluids). Then the samples
were subjected to tempering process. Tempering process, consists of reheating quenched steel
to a suitable temperature below the transformation temperature (400 and 550 oC) with a soaking
time were (30, 45 and 60min) and then allowed to cool down gradually.

2.6. Hardness testing

Before hardness tests were performed, all the heat treated specimen surfaces were ground and
polished for hardness measurement. Hardness was tested on all samples using (Jesus Miranda
Rockwell hardness tester), verified in accordance with (ASTM E18-14a). Rockwell Hardness
test was carried out at room temperature to measure the hardness of the medium carbon steel
specimens in (C scale). For each sample, four measurements were taken covering the whole
surface of the specimen and averaged was taken as final hardness results.
34 Abbas K. Hussein et al.

3. TAGUCHI METHOD
This is a statistical method also named as robust design method which has its wide applications
in most of the fields in recent times. This is a method developed by (Genichi Taguchi) to
improve the quality of all the manufactured goods in all the industries (Madhoo and Shilpa,
2017). The researchers introduced a unique concept known as Orthogonal Array which tries to
reduce the number of experimentation based on the trials by considering certain control
parameters (Thyla et al., 2015). Orthogonal Array provides a minimum number of
experimentations and Taguchi’s Signal to Noise ratio serves to give optimum results which are
based on the selection of the parameter (Shilpa and Naidu, 2010; Shilpa and Naidu, 2012). The
main application of this Taguchi’s method is implemented in the design of experiments (DOE)
(Shilpa,[Link] Naidu, 2014).

The Signal to Noise ratio can be calculated for three categories as below:

A. Larger the Better (LTB)

S
= −10log101/n ∑[1/Yi2 ] 2
N

B. Smaller the Better (STB)

S
N
= −10log10 ∑[Yi2 /n] 3

C. Nominal the Best (NTB)

S
N
= 10log10 ∑[Y 2 /S 2 ] (Madhoo and Shilpa, 2017)4 [13]

Where:

Y:results of experiments, observations or quality

N: Number of trials of repetitions.

S: the variance

4. SELECTION OF CONTROL FACTORS AND LEVELS

An appropriate orthogonal array for these experiments was selected. Here there are (5) factors
with (3) levels hence except tempering temperature with two levels as shown in the Table 3.

For this experimental (L18) orthogonal array is chosen. The (L18) orthogonal array has 18 rows
corresponding to the number of tests. Table 4 shows the 18 experiments supported (L18)
orthogonal array and their corresponding measured hardness. Replication technique has been
adopted to a void inaccuracy as shown in the Table 4.
 Kufa Journal of Engineering, Vol. 10, No. 1, January 2019 35

Table 3. Control factors and their levels.

Symbol Control factors Levels Unit

o
A Tempering temperature 400 550 ----- C
B Concentration media 0.01% 0.03% 0.08% -----
C base media Deionized water Salt solution Engine oil -----
D Nano particles type αAl2O3 TiO2 Cuo -----
E Tempering time 30 45 60 min

5. RESULTS AND DISCUSSIONS

5.1. S/N ratios analysis

The influence of control parameters on hardness was evaluated using(S/N) ratio response
analysis. The hardness characteristic selected was (larger is the better type) and the same type
of response was used for signal to noise ratio which is given above. The(S/N) ratio response
was analyzed using the Equation (2) for all fifty-four tests and presented in Table 4. The plots
in Figs. 2 and 3 shows the variation of individual response with the five parameters; tempering
temperature, the volume fraction of nanoparticles, type of base media, type of nanoparticles and
time tempering separately. The main effect plots are used to determine the optimal design
conditions to obtain high hardness.

Table 4. Signal to Noise Ratio for the controlling factors considering Hardness.

Parameters Trail Trail Trail

Expt. S/N Ratio
A B C D E (1) (2) (3)
1 400 0.01 Deionized water α-Al2O3 30 61 61 60 35.658210184
2 400 0.01 Salt Solution TiO2 45 58 58 58 35.268559871
3 400 0.01 Engine oil Cuo 60 56 57 57 35.065644549
4 400 0.03 Deionized water α-Al2O3 45 55 55 55 34.807253790
5 400 0.03 Salt Solution TiO2 60 59 58 59 35.366980613
6 400 0.03 Engine oil Cuo 30 57 57 57 35.117497113
7 400 0.08 Deionized water TiO2 30 56 58 59 35.212332444
8 400 0.08 Salt Solution Cuo 45 58 58 58 35.268559871
9 400 0.08 Engine oil α-Al2O3 60 53 52 54 34.482424494
10 550 0.01 Deionized water Cuo 60 41 41 41 32.255677134
11 550 0.01 Salt Solution α-Al2O3 30 42 44 45 32.792208535
 36 Abbas K. Hussein et al.

12 550 0.01 Engine oil TiO2 45 45 44 47 33.118622012

13 550 0.03 Deionized water TiO2 60 47 45 45 33.186538668
14 550 0.03 Salt Solution Cuo 30 45 45 45 33.064250276
15 550 0.03 Engine oil α-Al2O3 45 44 45 44 32.933149227
16 550 0.08 Deionized water Cuo 45 42 42 42 32.464985808
17 550 0.08 Salt Solution α-Al2O3 60 45 45 45 33.064250276
18 550 0.08 Engine oil TiO2 30 48 50 46 33.609727610

Table 5. Response table for (S/N) ratio.

Factor A FactorB Factor C Factor D Factor E

Level 1 35.138607 34.026487 33.93083 33.95625 34.24237
Level 2 32.9432677 34.0792783 34.13747 34.29379 33.97686
Level 3 34.0170468 34.05451 33.87277 33.90359
Delta 2.19533926 0.06223153 0.206635 0.421024 0.338785
Rank 1 5 4 2 3

Table 6. Response table of hardness for mean.

Factor A FactorB Factor C Factor D Factor E

Level 1 57.18518519 50.88888889 50.33333333 50.277778 52
Level 2 44.44444444 50.94444444 51.38888889 52.222222 50.4444444
Level 3 50.61111111 50.72222222 51.055556 50
Delta 12.74074074 0.333333333 0.388888889 1.9444444 2
Rank 1 5 4 3 2
 Kufa Journal of Engineering, Vol. 10, No. 1, January 2019 37

34.08 % Volume fraction of nanoparticles Tempering temperature

35.0
34.07

Mean of SN ratios
Mean of SN ratios

34.06 34.5

34.05
34.0
34.04

34.03 33.5

34.02
33.0
34.01
0.00 0.01 0.02 0.03 0.04 0.05 0.06 0.07 0.08 400 420 440 460 480 500 520 540 560

B A(℃)
Signal-to-noise:Larger is better Signal-to-noise:Larger is better

34.15
34.3 Tio2 Type of nanoparticles
Salt solution Base media

34.10
34.2
Mean of SN ratios

Mean of SN ratios

[Link] effects plot for (S/N) ratios – Hardness. Engine oil

34.05
34.1

34.00

34.0

α Al2o3 [Link] effects plot for (S/N)33.95ratios – Hardness.

33.9
Deionized water
Cuo
33.90

D c
Signal-to-noise:Larger is better Signal-to-noise:Larger is better

34.25 Tempering temperature

34.20
Mean of SN ratios

34.15

34.10

34.05

34.00

33.95

33.90

30 35 40 45 50 55 60

E(min)
Signal-to-noise:Larger is better

Fig. 2. Main effects plot for (S/N) ratios – Hardness.

38 Abbas K. Hussein et al.

57.5 Tempering temperature 50.95 % Volume fraction of nanoparticles

50.90
55.0

50.85
Mean of Means

Mean of Means
52.5
50.80

50.0 50.75

50.70
47.5

50.65
45.0
50.60
400 420 440 460 480 500 520 540 560 0.00 0.01 0.02 0.03 0.04 0.05 0.06 0.07 0.08

A(℃) B

51.50 Base media 52.5 Type of nanoparticles

Salt solution Tio2

51.25 52.0
Mean of Means

Mean of Means

51.00 51.5

Cuo
Engine oil 51.0
50.75

50.5
50.50
α Al2o3
Deionized water
50.0
c D

52.0 Tempering time

51.5
Mean of Means

51.0

50.5

50.0

30 35 40 45 50 55 60

E( min )

Fig. 3. Main effects plot for means- Hardness.

 Kufa Journal of Engineering, Vol. 10, No. 1, January 2019 39

From the response Table 5 and Fig. 2, it is clear that tempering temperature is the most
influencing factor followed by nanoparticles type then tempering time, subsequently type of
base media and percentage of nanoparticles is located in ranked last. Also, the results show that
the effect of the salt solution as base media was higher than deionized water and engine oil, in
addition to the (0.03%) volume fraction of nanoparticles and (TiO2) nanoparticles have higher
effects on the hardness.

5.2. Analysis of variance

The Table 7 shows analysis of variance for the hardness value of the medium carbon steel. From
Table 7, it is observed that the tempering temperature, percentage of nanoparticles, base media,
type of nanoparticles and tempering time affect the hardness of medium carbon steel. The last
column of the Table 7 indicates the percentage contribution of each other on the total variation
indicating their degree of effect on the result. It can be observed from the (ANOVA) table that
the tempering temperature (89.880%) was the most significant parameter on the hardness of
medium carbon steel followed by type of nanoparticles (2.234%) then tempering time (1.628%)
next base media (0.420%) and the least affected was percentage of volume fraction of
nanoparticles (0.0471%). The pooled error associated in the (ANOVA) table was approximately
about (5.789%) for hardness. This approach gives the variation of means and variance to
absolute values considered in the experiment and not the unit value of the variable.

Table 7. Results of the (ANOVA).

Source DF SeqSS AdjMS F-value P-Value Percentage of contribution

A 1 2191 2191 683.13 0 89.88003199

B 2 1.15 0.57 0.18 0.837 0.047166909
C 2 10.26 5.13 1.6 0.214 0.420810861
D 2 54.48 27.24 8.49 0.001 2.234481061
E 2 39.7 19.85 6.19 0.004 1.62828374
Error 44 141.2 3.21 5.789225437
Lack –of-Fit 8 111.8 13.98 17.15
Pure Error 36 29.33 0.81
Total 53 2438 100

5.3. Regression Equation

 40 Abbas K. Hussein et al.

A Regression model is developed using statistical software (MINITAB17). This model gives
the relationship between an independent/predicted variable and a response variable by fitting
linear equations to observe data. Regressions equation thus generate correlations between the
significant terms obtained from (ANOVA) analysis namely tempering temperature, the
percentage of the volume fraction of nanoparticles, base media, type of nanoparticles and
tempering time. The regression equations developed for hardness were shown in the Table 8.

Table 8. The regression equations for hardness.

Quenching media Type of nano particles Regresision equations

(HRC) = 92.99 - 0.08494 Tempering temperature
Deionized water Cuo
- 4.49 %of nanoparticles - 0.0667 tempering time
(HRC) = 95.27 - 0.08494 Tempering temperature
Deionized water TiO2
- 4.49 %of nanoparticles - 0.0667 tempering time
Deionized water (HRC) = 93.32 - 0.08494 Tempering temperature
α-Al2O3
- 4.49 %of nanoparticles - 0.0667 tempering time
(HRC) = 93.38 - 0.08494 Tempering temperature
Engine oil Cuo
- 4.49 %of nanoparticles - 0.0667 tempering time
(HRC) = 95.65 - 0.08494 Tempering temperature
Engine oil TiO2
- 4.49 %of nanoparticles- 0.0667 tempering time
(HRC) = 93.71 - 0.08494 Tempering temperature
Engine oil α-Al2O3
- 4.49 %of nanoparticles- 0.0667 tempering time
(HRC) = 94.04 - 0.08494 Tempering temperature
Salt Solution Cuo
- 4.49 %of nanoparticles- 0.0667 tempering time
(HRC) = 96.32 - 0.08494 Tempering temperature
Salt Solution TiO2
- 4.49 %of nanoparticles - 0.0667 tempering time
(HRC) = 94.38 - 0.08494 Tempering temperature
Salt Solution α-Al2O3
- 4.49 %of nanoparticles- 0.0667 tempering time

5.4. Model Summary

The summary of the model can be illustrated in Table 9.

Table [Link] summary.

S R-sq R-sq(adj) R-sq(pred)

1.77579 94.05% 93.15% 91.60%
 Kufa Journal of Engineering, Vol. 10, No. 1, January 2019 41

Fig. 4. Normal probability plot of residuals (hardness).

The graphs show that the data closely follow the straight lines, denoting a normal distribution.
Also, it can be observed from regression equations that the coefficient associated with
tempering temperature, Percentage of the volume fraction of nanoparticles, Base media, Type
of nanoparticles and tempering time are negative that indicates the hardness of the material
decrease with increasing the above parameter.

6. CONCLUSIONS
The approach of (Taguchi‘s) robust design method to hardness study led to conclude the
following:

A- Taguchi method provides a systematic and efficient methodology for the design and
optimization of quenching of nanofluids and tempering heat treatment parameters to maximize
hardness with far less effort than would be required for most optimization techniques.

B- From response table for (S/N)ratio with respect to the hardness (LTB) it is clear that
tempering temperature is the most significant factor influencing hardness followed by type of
nanoparticles then type of nanoparticles next tempering time then type of base media and
percentage of volume fraction of the nanoparticles which is the least significant factor.

C- The analysis of variance shows that the percentage contribution of tempering temperature,
percentage of volume fraction of nanoparticles,base media,nanoparticles type and tempering
time are (89.880%),(2.234%),(1.628%),(0.420%),(0.0471%)respectively.

The d-the pooled error associated with the (ANOVA) analysis was (5.789%) for hardness, and
the correlation between the hardness parameters was obtained by multiple linear regression
models.
42 Abbas K. Hussein et al.

E-The important sequence of optimal conditions for hardness is tempering temperature, type of
nanoparticles, tempering time Base media, the percentage of the volume fraction of
nanoparticles.

F-The optimal parameters for hardness value are tempering temperature (400oC), (0.03%)
volume fraction of nanoparticles, the salt solution as base media, type of nanoparticles (TiO2)
and tempering time (30min).

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