Available online at www.scholarsresearchlibrary.

com

Scholars Research Library

European Journal of Applied Engineering and
Scientific Research, 2012, 1 (4):235-240
(http://scholarsresearchlibrary.com/archive.html)

ISSN: 2278 – 0041

Synthesis, characterization of TiO2 nano powder and water based nanofluids using two
step method

Kavitha T 1, Rajendran A2, Durairajan A3

1
Department of Physics, Nehru Memorial College, Puthanampatti, Tiruchirapalli, Tamilnadu, India.
2
Department of Physics, Nehru Memorial College, Puthanampatti, Tiruchirapalli, Tamilnadu, India.
3
Department of Mechanical Engineering, K.S.R. College of Engineering, Tiruchengode, Tamil Nadu,
India.
________________________________________________________________________________________

ABSTRACT

This paper summarizes some of our recent research work on the synthesis of nanofluids (dilute liquid suspensions of
nanoparticles). In the present work, Tio2 Nano particles have been synthesized by Sol-gel technique. The Prepared
powders were characterized by using XRD, SEM. The Crystalline size of TiO2 powder was found to ~6 nm for
anatase at 400 ºC by controlling the acidity. TiO2 water nanofluids with different volume concentrations from 1% to
2% were then prepared by dispersing the synthesized Nano particles in deionised water.

Key words: Nano Tio2, Nano particles, SEM, XRD, Nano fluids.
_____________________________________________________________________________________________

INTRODUCTION

Nanofluids are a new class of fluids engineered by dispersing nanometer-sized materials (nanoparticles, nanofibers,
nanotubes, nanowires, nanorods, nanosheet, or droplets) in base fluids. Common base fluids include water, organic
liquids (e.g. ethylene, tri-ethylene-glycols, refrigerants, etc.), oils and lubricants, bio-fluids, polymeric solutions and
other common liquids. Materials commonly used as nanoparticles include chemically stable metals (e.g. gold,
copper), metal oxides (e.g., alumina, silica, zirconia, titania), oxide ceramics (e.g. Al2O3, CuO), metal carbides (e.g.
SiC), carbon in various forms (e.g., diamond, graphite, carbon nanotubes, fullerene) and functionalized
nanoparticles [1-5]. Nanofluids can be prepared by a one-step or a two-step method. In the two-step method in
which nanoparticles or nanotubes are first produced as a dry powder [3] and then dispersed into a fluid in a second
processing step [39-41]. In view of the synthetic methods developed for the preparation of nanostructure TiO2, a
wide variety of approaches including flame synthesis , ultrasonic irradiation, chemical vapor deposition, sol–gel
Method. Among them, Compared to other methods, sol-gel route is regarded as a good method to synthesis ultra-
fine metallic oxide and has been widely employed for preparing titanium dioxide (TiO2) particles [42, 43]. TiO2
water nanofluids with different volume concentrations from 1% to 2% were then prepared by dispersing the
synthesized Nano particles in deionised water and particles size was found to be ~6nm [5,6]. Thermal conductivities
of various solids and liquids are listed in table 1.

235
Scholars Research Library
Kavitha T et al Euro. J. Appl. Eng. Sci. Res., 2012, 1 (4):2
(4):235-240
______________________________________________________________________________
Table1: Thermal conductivity of various solids and liquids

Material Thermal conductivity (W/mK)

mK)
Nanotubes 1800-6600
Diamond 2300
Carbon Graphite 110-190
Fullerenes film 0.4
Metallic solids (pure) Copper 401
Aluminum 237
Nonmetallic solids Silicon 148
Alumina (Al2O3) 40
Metallic liquids Sodium (644 K) 72.3
Nonmetallic liquids Water 0.613
Ethylene glycol (EG) 0.253
Engine oil (EO) 0.145

MATERIALS AND METHODS

2. Experimental Study
2.1 Synthesis
ynthesis and preparation methods
The Preparation of nanofluids is the first key step in experimental studies with nanofluids.

2.1.1 Two step technique

Two-step
step method is the most widely used method for preparing nanofluids. Nanoparticles,
Nanoparticles nanofibers, nanotubes,
and nanomaterials. In this method, first produced as dry powders by using chemical or physical methods [6-9]. We
used sol gel technique for preparation of nano Tio2 powders [8].. The obtained nanosized powder will be dispersed
into a base fluid (Water) in the second processing step with the help of intensive magnetic force agitation.

2.1.2 Nano Tio2 preparation by using sol gel technique

TiO2 Nano-powders
powders were prepared via sol–gel
sol gel method using titanium tetraisopropoxide (TTIP, Merck), distilled
water, ethyl alcohol (EtOH, Merck) as the starting materials. Titanium tetraisopropoxide was dropped slowly into
the solution of water and ethyl alcohol while
while magnetic agitating continuously to get white slurry solution [36]. The
obtained solutions were kept under slow-speed
slow speed constant stirring on a magnetic stirrer for 40mins at room
temperature [12].. Then the precipitated TiO2 was filtered and dried at 50ºC for 1 h until it was turned into white
block crystal. After ball milling the dried powders obtained were calcinated at 400ºC for 2 h to observe the phase
changes accompanying the heat treatments [10-12].

2.2 Nanofluids preparation using Tio2 nanoparticles

The TiO2 Nano particles have an average size of 6 nm used for investigation in the present experimental work. The
photographic view of the nanoparticles as seen by the naked eyes is shown in the Figure 2.1 [12, 13]. The
distribution of TiO2 nanoparticles at Nano scale can be observed under a Scanning Electron
lectron Microscope (SEM). The
SEM images of TiO2 nanoparticles as shown in the figure 3.2 [35-37].. Preparation of nanofluids is an important
stage and nanofluids are prepared
pared in a systematic and careful manner [13-16].. A stable nanofluid with uniform
particle dispersion is required and the same is used for measuring the thermo physical properties of nanofluids [17].

Figure 2.1: Photographic view of Tio2 nanoparticles

236
Scholars Research Library
Kavitha T et al Euro. J. Appl. Eng. Sci. Res., 2012, 1 (4):235-240
______________________________________________________________________________
In this method a small amount of suitable surfactant, generally one tenth of mass of nanoparticles, is added to the
base fluid and stirred continuously for few hours. Nanofluids prepared using surfactants will give a stable
suspension with uniform particle dispersion in the host liquid [18, 19]. The nanoparticles remain in suspension state
for a long time without settling down at the bottom of the container [30].

After estimate the amount of nanoparticles required for preparation of TiO2 Nanofluids for a given volume
concentration [20]. Nanoparticles are mixed in the base fluid of water [31-33]. In the present investigation, neither
surfactants nor acid are added in the TiO2 nanofluids, because with the addition of surfactants the thermo physical
properties of nanofluids are affected [20-22].

Addition of acid may damage the tube material because corrosion takes place after a few days with the prolonged
usage of such nanofluids in practical applications [22]. All the test samples of TiO2 nanofluids used subsequently for
estimation of their properties were subjected to magnetic stirring process followed by ultrasonic vibration for about
2 hours [23-25]. The photographic view of TiO2 nanofluids sonication process using a Ultrasonic Cleaner is shown
in the figure 2.2

Figure 2.2: Ultrasonic Cleaner apparatus for sonication process of TiO2 Nanofluids

The TiO2 nanofluids samples thus prepared are kept for observation and no particle settlement was observed at the
bottom of the flask containing TiO2 nanofluids even after 3 hours .[24-28] The photographic view of TiO2
nanofluids suspension prepared after magnetic stirring and sonication process is as shown in Figure 2.3

Figure 2.3: The photographic view of Tio2 nanofluids suspension

237
Scholars Research Library
Kavitha T et al Euro. J. Appl. Eng. Sci. Res., 2012, 1 (4):235-240
______________________________________________________________________________
RESULTS AND DISCUSSION

Figure 3.1: XRD Patterns of Titania particles calcinated at 4000c

3.1 Calcination temperature

Powder X-ray diffraction (XRD) as shown in figure 3.1and it was used for identification of crystalline phases and
estimation of the crystallite size. The X-ray diffraction (XRD) patterns were performed on a Seimens/ D5000 X-ray
diffractometer. From the line broadening of corresponding X-ray diffraction peaks and using the Scherrer formula
the crystallite size, L has been estimated.

L =Kλ /(β cos θ)

where λ is the wavelength of the X-ray radiation (Cu Kα = 0.15406 nm), K is a constant taken as 0.89, β is the line
width at half maximum height, and θ is the diffracting angle. The surface morphology of the calcinated powders at
400ºC was observed on scanning electron microscopy (SEM).

3.2 SEM Morphology

The morphology of calcinated titania powders at 400ºC observed by SEM is shown in Fig. 3.2. The size of titania
particles was about 6 nm and non hard-grained aggregates that are constituted of sharp faceted nanoscaled crystals
were formed [28-30].

238
Scholars Research Library
Kavitha T et al Euro. J. Appl. Eng. Sci. Res., 2012, 1 (4):235-240
______________________________________________________________________________

3.2 SEM Morphology of calcinated titania powder at 4000c

CONCLUSION

Nanofluids, i.e., well-dispersed metallic nanoparticles at low volume fractions in liquids, enhance the mixture’s
thermal conductivity over the base-fluid values. Thus, they are potentially useful for advanced cooling of micro-
systems. In summary, Nano- TiO2 powders have been prepared by sol-gel method and found to be 6nm. The future
scope in the nanofluids research cycle are to concentrated on heat transfer enhancements and determine its physical
mechanisms, taking into consideration such items as the optimum particle size and shape, particle volume
concentration, fluid additive, particle coating, and base fluid. TiO2 water nanofluids with different volume
concentrations from 1% to 2% were then prepared by dispersing the synthesized Nano particles in deionised water.

Acknowledgments
We are thankful to principal, professors and lecturers, technical and non-technical staff those who are supported for
the proposed research in the Department of Physics and Mechanical Engineering.

REFERENCES

[1] H. Akoh, Y. Tsukasaki, S. Yatsuya, A. Tasaki, Journal of Crystal Growth 45 (1978) 495–500.
[2]Choi SUS. Developments and applications of non-newtonian flows. In: Siginer DD, Wang HP, Eds. American
Society of Mechanical Engineering, New York 1995; 231(66): 99.
[3]Cheng L, Bandarra FEP, Thome JR. J Nanosci Nanotech 2008; 8: 3315.
[4]Keblinst.P, Eastman.J.A and Cahill.D.G, Materials Today, 8 (2005), 6, pp. 36-44.
[5] Keblinst.P, Phillpot.S.R, Choi.S.U.S, and Eastman.J.A, International Journal of Heat and Mass Transfer,
45(2002), 4, pp. 855-863.
[6]Eastman.J.A,Cho.S.U.S,Li.S,Thompson.L.J,and Lee.S, “Enhanced thermal conductivity through the development
of Nanofluids”, Fall meeting of the Materials Research Society,Boston, USA,1997.
[7]Masuda.H,Ebata.A, Teramae.K and Hishinuma.N, Netsu Bussei, 7 (1993), pp. 227 – 233.
239
Scholars Research Library
Kavitha T et al Euro. J. Appl. Eng. Sci. Res., 2012, 1 (4):235-240
______________________________________________________________________________
[8] Lee.S,Choi.S.U.S and Eastman.J.A Transactions of ASME Journal of heat transfer, 121 (1999), 2, pp. 280 - 289.
[9]Pak.B.C and Cho.Y.I, Experimental Heat Transfer, 11 (1998), 2, pp. 151 – 170.
[10]Das.S.K., Putra. N., Thiesen.P and Roetzel.W, Transactions of the ASME Journal of Heat Transfer, 125 (2003),
4, pp. 567-574.
[11] Xie, H. WangJ; xi T.; liu Y.; Ai,F; Wu.Q Journal of Applied Physics,91 (2002), 7, pp. 4568-4572.
[12] Prasher R, Phelan.P.E and Bhaltacharya.P Nanoletters, 6 (2005), 7, pp. 1529 – 1534.
[13] Murshed.S.M.S,Leong.K.C and Yang.C, International Journal of Thermal Sciences, 44 (2005), 4, pp. 367 –
373.
[14] Krishnamuthy.S, Bhattacharaya.P, Phelen P.E and Prasher.R.S Nano Letters, 6 (2006), 3, pp. 419-423.
[15] Liu.M.S, Lin.C.C, Haung.I.T and Wang C.C, Chemical Engineering and Technology, 29 (2006), 1, pp. 72- 77.
[16] Wenhua. Yu, David m. France, Jules .L. Routbort, and Stephen U.S.Choi, Heat Transfer Engineering, 29
(2008), 5, pp. 432-460.
[17] S.Zeinali Heris, S.G. Etemad, M. Nasir. Esfahany, International Journal of Heat and Mass Transfer, 33 (2006),
pp. 529-535.
[18] Wen D and Ding Y, International Journal of Heat & Mass Transfer, 47 (2004), pp. 5185-5188.
[19] Yang Y, Zhang Z.G, Grulke E.A, Anderson WB, Wu.G, International Journal of Heat & Mass Transfer, 48
(2005), 6, pp. 1107-1116.
[20] Khanafer . K, Vatai. K and Lightstone. M International Journal of Heat & Mass Transfer”, 46 (2003), pp.
3639-3653.
[21] Kim.J, Kang Y.T and Choi.C.K, Physics of Fluids, 16 (2006), 7, pp. 2395-2401.
[22] Ulzie Rea, Tom Mckrell, Lin-Wen Hu, Jacop Buongiorno, International Journal of Heat & Mass Transfer,
52(2009), pp. 2042-2048.
[23] H. B¨onnemann, S. S. Botha, B. Bladergroen, and V. M. Linkov, Applied Organometallic Chemistry, vol. 19,
no. 6, pp. 768–773, 2005.
[24] A. K. Singh and V. S. Raykar, “Colloid and Polymer Science, vol. 286, no. 14-15, pp. 1667–1673, 2008.
[25] A. Kumar, H. Joshi, R. Pasricha, A. B. Mandale, and M. Sastry, Journal of Colloid and Interface Science, vol.
264, no. 2, pp. 396–401, 2003.
[26] W. Yu, H. Xie, X. Wang, and X. Wang, Nanoscale Research Letters, vol. 6, p. 47, 2011
[27] Maxwell J.C. (1873) A treatise on electricity and magnetism, Clarendon Press, Oxford, UK.
[28] Bang I.C. and Chang S.H. (2005) International Journal of Heat and Mass Transfer 48, 2407-2419
[29] Xie H., Wang J., Xi T. and Liu Y. (2002b) International Journal of Thermophysics, 23, 571-580
[30] X. Feng, H. Ma, S. Huang et al., Journal of Physical Chemistry B, vol. 110, no. 25, pp. 12311–12317, 2006.
[31] Das, S. K., Putra, N., and Roetzel,W., International Journal of Multiphase Flow, 29(2003), pp. 1237–1247.
[32] Wen, D., and Ding, Y., Journal of Nanoparticle Research, 7 (2005), pp. 265– 274.
[33] Liu, Z.-H., and Qiu, Y.-H., Heat and Mass Transfer, 43 (2007), pp. 699–706.
[34] Wehua Yu, David M. France, Jules I. Routbort and Stephan U.S. Choi, Heat Transfer Engineering, 29 (2008),
5, pp. 432-460.
[35] Yang B. and Han Z.H. (2006) Applied Physics Letters, 89, 083111.
[36] M. Chopkar, I. Manna, P.K. Das (2008). Heat and Mass Transfer, vol 44: pp 999–1004.
[37] M. Chopkar, P. K. Das and I. Manna (2006). Synthesis and Characterization of Nanofluid for Advanced Heat-
Transfer Applications Scripta Materialia, Vol 55: pp 549–552.
[38] M. Chopkar, P. K. Das and I.Manna (2007). Mater. Sci. Eng. B, vol 139: 141–148
[39] K. V. Wong and O. de Leon, Advances in Mechanical Engineering, vol. 2010, Article ID 519659, 11 pages,
2010.
[40] S.K. Das, N. Putta, P. Thiesen, W. Roetzel, ASME Trans. J. Heat Transfer 125 (2003) 567–574.
[41] Y. Nagasaka, A. Nagashima, Journal of Physics E: Scientific Instruments 14 (1981) 1435– 1440.
[42] G. Donzelli, R. Cerbino, and A. Vailati, Physical Review Letters, vol. 102, no. 10, Article ID 104503, 2009.
[43] M. Arruebo, R. Fern´andez-Pacheco, M. R. Ibarra, and J. Santamar´ıa, Nano Today, vol. 2, no. 3, pp. 22–32,
2007.
[44] W. Yu, D. M. France, D. Singh, E. V. Timofeeva, D. S. Smith, and J. L. Routbort, Journal of Nanoscience and
Nanotechnology, vol. 10, no. 8, pp. 4824–4849, 2010

240
Scholars Research Library