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In this project we have found that the XRD pattern of the TiO2 nano particles, the peaks are observed at corresponding values. The SEM images of TiO2 nano particles shows respectable morphology and Grain size of TiO2 nano particles were nearly 60.03 nm. The Energy dispersive X-ray spectroscopy reveals that the required phase has present. Titanium and oxygen (O) Elements are present in the sample. The grain structure and size were nearly 240 nm. TiO2 Coated nano particles on mild steel at 500° C, shows respectable morphology when compared with base metal of the sample and grain size of coated sample 500° C were nearly 204 nm. Initially the surface roughness of the base metal is high when compared with heat treated sample at 500°C due to the heat treatment the surface roughness of the sample is smooth. Surface roughness is high after deposition of Tio2 nano particles on mild steel at 500°C, due to high bond generated between Tio2 and mild steel during dipping process.
ABSTRACT:
In this project we have found that the XRD pattern of the TiO2 nano particles, the peaks are observed at corresponding values. The SEM images of TiO2 nano particles shows respectable morphology and Grain size of TiO2 nano particles were nearly 60.03 nm. The Energy dispersive X-ray spectroscopy reveals that the required phase has present. Titanium and oxygen (O) Elements are present in the sample. The grain structure and size were nearly 240 nm. TiO2 Coated nano particles on mild steel at 500° C, shows respectable morphology when compared with base metal of the sample and grain size of coated sample 500° C were nearly 204 nm. Initially the surface roughness of the base metal is high when compared with heat treated sample at 500°C due to the heat treatment the surface roughness of the sample is smooth. Surface roughness is high after deposition of Tio2 nano particles on mild steel at 500°C, due to high bond generated between Tio2 and mild steel during dipping process.
KEYWORDS: TiO2 nano particles, mild steel, XRD and SEM analysis.
1.INTRODUCTION:
Nanotechnology literally means any technology on a nanoscale that has applications in the real world. The nanotechnology in mechanical engineering and manufacturing is immensely useful to the field. Nanotechnology can be used to increasing the life of the components and automobile parts. A many number of materials can be enhanced by the use of nanotechnology. In this paper they focused on deposition of Al2O3 nano particles on steel by machining process and heat treatment process. A considerable difference in hardness is achieved after deposition. Surface roughness is lowered after deposition. Xinkun Suoa et al stated that microstructure, phase structure, oxygen content and micro hardness of the coating prepared under different main gas temperatures were investigated. The critical velocity of the particle was evaluated through numerical simulations [1]. M.Sneha-P. Sammaiah et al stated that The particle deformation behaviour and bonding mechanism were discussed. The result of the oxygen content test showed that the oxygen contents of the coatings did not increase comparing with that of the feedstock powder. The simulation results revealed that the critical velocity of Mg particles was in a range of 653 m/s to 677m/s [2]. The paper investigated on microstructure evolution as a function of basic spray parameters temperature and pressure onto AA6060 aluminium alloy and 1.0037 steel substrates was studied. Adherent and dense 50-80 pm thick Ti2AlC coatings were deposited on soft AA6060 substrates under gas temperature and pressure of 600°C and 3.4 MPa, respectively, whilst comparable results were obtained on harder 1.0037 steel by using higher temperature (800°C) and pressure (3.9 MPa) [3]. Jon affi et al stated that the cold spray process for developing a metallic coating technique. In this study, aluminum coating was fabricated onto the carbon fiber-reinforced plastic (CFRP) substrate using interlayer. It was difficult to fabricate the cold-sprayed aluminum coating directly on the CFRP substrate. Though smaller size aluminum particles could be deposited on the CFRP substrate, but the coating was peeled off when the thickness was around 30 pm. The interlayer with larger contact area could retain on the substrate and able to facilitate the deformation of the next incoming cold- sprayed particles to build a thick coating. The volume resistivity of cold spray coating is lower than the plasma sprayed aluminum coating because the high process gas temperature in the latter case enhances the oxidation of sprayed particle. Therefore, a lower process gas temperature should be used to fabricate lower volume resistivity coating on cold spray [4]. N.H.N Musoffa et al stated that, this paper discusses the effect of plasma spray parameters of deposited agglomerated nano Al2O3- 13% TiO2 powders on commercial marine-grade mild steels. These operational spray parameters potentially affect the following responses of the coatings: micro hardness, wear rate, and surface roughness. The significant effect on surface roughness is due to the interaction factor with the carrier gas pressure. However, by changing the carrier gas pressure and the powder feed rate, an insignificant effect on the micro hardness and wear rate is noted. In general, agglomerated Al2O3- 13%TiO2 nanopowder-coated steels, with the lowest primary pressure of 40 psi, carrier gas pressure of 20 psi, and the highest powder feed rate of 3 rpm, are most preferred [5]. Y. wang, S. Limb et al stated that the tribological and electrochemical corrosion properties of Al2O3/polymer nanocomposite coatings were studied by using micro-hardness test, single-pass scratch test, abrasive wear test, and finally electrochemical technique such as potentiodynamic polarization measurement. The improvement in scratch and abrasive resistance is attributed to the dispersion hardening of Al2O3 nanoparticles in polymer coatings [6]. S. dong et al found that The coating exhibited uniform mechanical properties throughout its thickness, Nanoindentation was used to produce maps of the hardness and elastic modulus through cross-sections of a brush plated nanoparticle composite n-Al2O3/Ni coating on mild carbon steel. The Young's modulus of the brush plated n-Al2O3/Ni composite coating was ~200 GPa [7-8]. In this investigation a uniform TiO2 nanoparticle coating has been applied on mild steel, using sol-gel method. The coating was deposited on mild steel substrate by dip coating technique. The morphology and structure of the coating were analyzed using SEM, AFM and X-ray diffraction. The anticorrosion performances of the coating have been evaluated by using electrochemical techniques. The Tafel polarization measurements provide an explanation to the increased resistance of TiO2 nano particle coated mild steel against corrosion and icorr was decreased from 18.621 to 0.174pA/cm2.
2.EXPERIMENTAL DETAILS:
Material Used:
* Tio2 nano particles
* Mild steel plate (10 x 15 x 2 mm)
* Titanium Isopropoxide: (C12H28O4Ti)
* Ethanol :C2H5OH 50 mL
* H2O 200 mL
2.1SYNTHESIS OF Tio2 NANO PARTICALS USING SOLUTION COMBUTION PROCESS:
Ethanol and titanium tetrachloride were introduced into a beaker; the solution was stirred for 30 min. During this period, it formed a yellow sol phase. Bi distilled water was added and the solution became clear and colorless. The solution was again stirred for 30 min at room temperature and then the formed gel was dried at 50 °C for 24 h.
(C12H28O4TO+ C2HsOH^ TiO2+H2O|+CO2Î+CO
2.2OPERATIONS:
(i) Specimens Preparation:
To perform the experimental test the mild steel specimen is prepared by the following steps
(ii) Cutting:
As the convinces of experimental analysis and Surface condition of specimen is considered as an important factor it is necessary to prepare a uniform surface. Square specimens were obtained as a final specimen shape. 10·10mm.
(iii) Polishing:
The specimens were polished using polish cloth and alpha alumina 1 pm and 0.5 pm, and then washed with distilled water. The polished specimens were dried and tested for material composition by using EDX.
2. 3 Experimental Procedure:
Sample and solution preparation Figure shows the mild steel sample used in this experiment. The steel was mechanically cut into square shape using machining process with thickness of 3 mm and 10·10mm. For dip-coating purpose, 1 mm hole was drilled on the top of the sample. After that, the sample was polished by emery paper until 800 grit and cleaned by acetone. For sol-gel solution, Ethanol and titanium tetrachloride were introduced into a beaker the solution was stirred for 30 min., ethanol, and distilled water were prepared at fixed molar ratio of1:3.2. Then acetone was added to the mixture continued to stir for another 30 minutes. Distilled water then added to continue for another 30 minutes.
2. 4 Coating Technique:
The substrates were fully immersed in titanium tetrachloride solution for 10 minute after which air dried for another 2 minutes. These steps were repeated according to the number of coatings of each substrate. Once the deposition of the coating was completed, the substrates were thermally treated. During this phase, excess organic compounds found on the surface of coated substrates will evaporate. The substrate then annealed at 500°C for two hours in the muffle furnace.
3.RESULTS AND DISCUSSIONS:
3.1 X-RAY DIFFRACTION:
In the XRD pattem of the TiO2 nano particles, the peaks are observed at 30.577, 35.151, 37.777, 49.354, 57.501 and 63.211 (h k l) values of the peaks are (0 1 2), (1 0 4), (1 1 0), (1 1 3), (1 1 6) and (3 0 0)respectively. These results are coincided with JCPDS card number 82-1468, and it shows that the TiO2 nano particle consists of Spherical shaped structure. The average crystalline size is measured using Debye-Scherer's formula [5].
According to the Debye-Scherer's equation: (ProQuest: ... denotes formula omitted.)
Where D - Average size of the particle [nm]
Я -Wavelength of the radiation [A°]
0 -Diffraction angle [degree]
B - Full width half maximum (FWHM) of the peak [radians]
From the above formula obtained average crystalline size is 55 nm. The lattice parameter a = b = 4.7589 A°, c = 12.9919 A°.
3.2SCANNING ELECTRON MICROSCOPY:
SEM images of TiO2 nano particles and the grain size, shape and surface properties like morphology were observed by using SEM with different magnifications. The SEM images of TiO2 nano particles shows respectable morphology and Grain size of TiO2 nano particles were nearly 60.03 nm as shown in the figure 16.
3. 3 EDX OF TIO2 NANO PARTICLES:
The EDX of the sample was done by the SEM (HITACHI S3400NS) machine. The Energy dispersive X-ray spectroscopy reveals that the required phase has present. Titanium and oxygen (O) Elements are present in the sample as shown in the figure 17.
Spectrum processing: Peaks possibly omitted: 1.043, 2.830 keV
Processing option: All elements analyzed (Normalised)
Number of iterations = 2
Standard: O SiO2 1-Jun-1999 12:00 AM. Zr Zr 1-Jun-1999 12:00 AM
3.4 SEM IMAGES OF THE BASE METAL:
SEM images of the base metal as shown in the figure 18. The grain size, shape and surface properties like morphology were observed by the SEM with different magnifications. It shows coarse grain structure and size were nearly 240 nm.
3. 5 EDX OF BASE METAL:
The EDX of the sample was done by the SEM (HITACHI S3400NS) machine. The Energy dispersive X-ray spectroscopy reveals that the required phase has present. Carbon (C), oxygen (O) and iron (Fe) Elements are present in the sample as shown below.
3.6 SEM IMAGES OF COATED TIO2NANO PARTICLES ON MILD STEEL:
SEM images of coated TiO2 nano particles on mild steel at 500° C as shown in the figure 10. The grain size, shape and surface properties like morphology were observed by the SEM with different magnifications. Coated nano particles on mild steel at 500° C, shows respectable morphology when compared with base metal of the sample and grain size of coated sample 500° C were nearly 204 nm
3.7 Edx Of Coated Sample:
The EDX of the sample was done by the SEM (HITACHI S3400NS) machine. The Energy dispersive X-ray spectroscopy reveals that the required phase has present. Carbon (C), oxygen (O), iron (Fe) and Aluminium (Al) Elements are present in the sample as shown in the figure 21.
Spectrum processing: No peaks omitted
Processing option: All elements analyzed (Normalised)
Number of iterations = 3
Standard: C CaCO3 1-Jun-1999 12:00 AM
O SiO2 1-Jun-1999 12:00 AM
Na Albite 1-Jun-1999 12:00 AM
Fe Fe 1-Jun-1999 12:00 AM
TI TI 1-Jun-1999 12:00 AM
4. 8 SURFACE ROUGHNESS:
Initially the surface roughness of the base metal is high when compared with heat treated sample at 500°C due to the heat treatment the surface roughness of the sample is smooth. Surface roughness is high after deposition of Tio2 nano particles on mild steel at 500°C, due to high bond generated between Tio2 and mild steel during dipping process.
5. CONCLUSION:
TiO2 Nano particles are coated on the polished mild steel by using deposition technology then the samples is heat treated for the adhesion of TiO2 particles to the mild steel. And the sample is undergone for the XRD, SEM and Surface roughness analysis which are given good results. The surface roughness value for the coated mild steel is increased compare with the base material of mild steel. And in the SEM different magnifications observed that the TiO2 coated mild steel given respected morphology when compared to the base material.
6. REFERENCE:
1. Preparation and characterization of magnesium coating deposited by cold Spraying by Xinkun Suoa,·, Xueping Guoa, Wenya Li b, etc. © 2011 Elsevier B.V. Journal of Materials Processing Technology 212 (2012) 100- 105
2. Effect of Heat Treatment & Machining Process for Deposition of Al2O3 Nano Particles on Steel. M. Snehaa, Pulla Sammaiaha·,N. Sudheer Kumarb,S.P. Mrudulaa ,Mohd. Khaseema
3. Cold-spray deposition of Ti2AlC coatings S. Recha, A. Surpia·, S. Vezzú a, A. Patelli a, A. Trentin a, J. Glor b, J. Frodelius c,1, L. Hultman c . 2013 Elsevier Ltd. Vacuum 94.
4. Fabrication of Aluminum Coating onto CFRP Substrate by Cold Spray Jon Aff&0131;·, Hiroki Okazaki·, Motohiro Yamada and et al. (2011) Materials Transactions, Vol. 52, No. 9 (2011) pp
5. Optimization of plasma spray parameters on the mechanical properties of agglomerated Al2O3-13%TiO2 coated mild steel. 2012 Elsevier LtdMaterials and Design 39 (2012). N.H.N. Yusoff a, M.J. Ghazali b, M.C. Isa a, A.R. Daud c, A. Muchtar b, S.M. Forghani
6. Tribological and corrosion behaviour of Al2O3/polymer nanocomposite coatings Y. Wang a, S. Limb, J.L. Luob, Z.H. Xub (2006)
7. Determination of hardness and young's modulus of brush plated nano-al2o3/ni composite coating by nanoindentation testing. s. dong, b. d. beake, r. parkinson, b. xu, z. hu and t. bell
8. Mechanical properties of nanoparticles: basics and applications Dan Guo, Guoxin Xie and Jianbin Luo (2014). J. Phys. D: Appl. Phys. 47 (2014) 013001 (25pp). lop publications.
9. Corrosion Protection of Mild Steel by Applying TiO2 Nanoparticle Coating via Sol-Gel Method. A. Shanaghi, A. R. Sabour, T. Shahrabi, and M. Aliofkhazraee.
Copyright A&V Publications Jul-Sep 2019