SYNTHESIS AND CHARACTERIZATION OF TITANIUM METAL CARBON NANO TUBES

Transcription

1 International Journal of Nanotechnology and Application (IJNA) ISSN(P): ; ISSN(E): Vol. 4, Issue 3, Jun 2014, TJPRC Pvt. Ltd. SYNTHESIS AND CHARACTERIZATION OF TITANIUM METAL CARBON NANO TUBES UMA SHARMA 1 & B. TIWARI 2 1 Department of Chemistry, Mewar University, Rajasthan, India 2 D.S. Institutes of Technology and Management, Ghaziabad, Uttar Pradesh, India ABSTRACT The Carbon nanotubes have very vast applications due to many desirable properties. Carbon nanotubes have a number of extraordinary properties, high electric conductivity, high thermal conductivity, mechanical strength, thermal resistivity etc. The structure of carbon nanotubes can be visualized by rolling up a graphite sheet plane to a tube. The titanium carbon nanotubes are synthesized by a simple process of very low cost by using egg white proteins which acts as a gelling agent. The titanium carbon nanotubes are characterized by X-ray diffraction, FTIR results, thermo gravimetric analysis (TGA) X-ray diffraction analysis (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR) and ultra-violet (UV-visible). KEYWORDS: Ti (II) Albumin, CNTs, XRD, TEM, TGA, XRD, TEM, UV Visible Carbon Nanotubes Etc INTRODUCTION Various methods were introduced to synthesize titanium nanotubes. Some researchers suggest the micro emulsion method or the physical vapor method, or such as hydrolysis and hydrothermal have been used in many studies. However sol-gel method, the substance undergo hydrolysis and polycondensation processes to form the sol and then gel will be formed after aging or gelation and eventually become solid crystals after drying. This is the simplest and needs low temperature and gives high quality product. The appropriate size of titanium carbon nanoparticles can be obtained by using an egg white as the gelling agent. Egg white proteins (albumin) have high solubility in water and it associates with metal ions in solution. It works like a binder cum gel and gives proper shape to product. In this study, the characterization is done using X ray diffraction, scanning electron microscopy, UV/visible spectroscopy, transmission electron microscopy (TEM). Fourier transform infrared spectroscopies (FTIR) were also carried out at the range of cm 1, range of frequency. The sample was also subjected to thermo gravimetric analysis (TGA) to measure the thermal stability of the compound. Titanium carbon nanotubes are proved as good n-type semiconductors with high physical and chemical stability and high refractive index. It is widely used as photo catalyst, solar cells, sensors, self-cleaning, and bactericidal action Experimental Procedure Stoichiometric ratios of metal and ligands are dissolved in aqueous medium and are refluxed until the complex is precipitated, and if not, the ph of the solution mixture is changed to precipitate the complex. The Carbon Metal (Ti) Nano Tubes are synthesized by using egg Albumin and a one normal metal salt solution. The Titanium salt solution is allowed to react with amino acids present in egg albumin to form a complex of amino acids with Titanium ions. Albumin is proteinaceous in nature and is a polymer of amino acids. In amino acids, amino and carboxylic acid groups are attached on editor@tjprc.org

2 46 Uma Sharma & B. Tiwari both the sides of carbon chain. Both the ends then utilized for increasing the chain length and long carbon nano tubes are formed with the complex. The metal-albumin complex then decomposed at higher temperature to give carbon metal nano tubes. The synthesized complexes were found to be insoluble in the commonly known organic solvents. Consequently, the following physical measurements and analysis were carried out to check the purity and to elucidate the structure. All the metal complexes are stable to air and moisture and decompose at very high temperatures. Characterization of Titanium Carbon Nanoparticles The dried sample is subjected to TGA, Bruker-D8 Advance Powder X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FTIR) studies were carried out in the cm 1 frequency range, the infrared absorption spectra and UV-visible absorption spectrum.tga analysis measure the thermal stability of the sample.xrd is used to determine the crystal phase and crystalline size. Morphology and the particle size was measured using TEM and SEM.FTR, IR and UV gives the qualitative information of the bonding type and structural information of the sample. RESULTS AND DISCUSSIONS Module TG/DTA Channel 3 Data Name A-Uma -1 Measurement Time 4/29/ :22:21 AM Sample Name Sample-1 Table 1 Sample Weight mg Reference Name Alumina Powder Reference Weight 10.5 mg Temperature Cel Cel Cel/min min s Gas1 Gas2 Store Program Off On On Operator Name Organization Name Comment Surface Area DTA No. Temperature Program Mode A. K.Saini IIC Operator: A. K.Saini Gas1: Nitrogen (200ml/min) Gas2: Pan: Alumina Inst No. 1 DTA Area mj/mg Ramp Impact Factor (JCC): Index Copernicus Value (ICV): 3.0

3 Synthesis and Characterization of Titanium Metal Carbon Nano Tubes 47 Table 2 Time Temp. DTA TG DTG min Cel uv ug ug/min editor@tjprc.org

4 48 Uma Sharma & B. Tiwari Table 2: Contd., Thermo Gravimetric Analysis In TGA, the samples are heated and the losses in weights were observed. The first weight loss occurs at nearly 100 o c which is due to loss of water from the sample. The other loss of weight was due to evaporation of voltaic impurities like CH 3 COOH etc. There is no loss of weight between o c and it shows the stabilization of titanium carbon nanotubes. The fluctuation in the curves shows the, burning of different organic material in the protein of the sample. DTG curves consist of broad peak indicating the purification and the stability of the sample on heating. Differential Thermal Analysis (Or DTA) It is a is a thermo analytic technique and a DTA curve provides data on the transformations that have occurred, such as glass transitions, crystallization, melting and sublimation. The area under a DTA peak is the enthalpy change and is not affected by the heat capacity of the sample. The loss of the species on the surface of titanium carbon nanotubes is observed at 400 deg C and that shows that at this temperature most of the organic impurities are removed. Impact Factor (JCC): Index Copernicus Value (ICV): 3.0

5 Synthesis and Characterization of Titanium Metal Carbon Nano Tubes 49 Powder X Ray Diffraction Figure 1 X Ray diffraction helped in estimating the crystalline size for titanium CNTs. The size was estimated to be approximately 11nm to 18nm. The X ray diffraction peaks were in the wide angle range of 2Ѳ. Figure 2 editor@tjprc.org

6 50 Uma Sharma & B. Tiwari The crystalline size was calculated using 101 planes. Ѳ = o Scherrer s Equation D = K λ / β Cos Ѳ Λ Wavelength K is constant Β Half maximum height of the peak. Ѳ Diffraction angle. D crystalline size Transmission Electron Microscopy (TEM) Titanium CNT particles were dispersed in distilled water and tested ultrasonically. It was dropped on the Copper grid of transmission electron microscopy. The histogram shows the main particle size of Titanium CNT. It was around nm. Fourier Transforms Infrared Spectroscopy (FTIR) Figure 3 The range of FTIR is cm 1.The absence of peaks after 2900 cm 1 indicates the absence of organic carbon hydrogen stretches cm 1 is the stretch due O-H of the water which is absorbed on the surface of the sample. 485 cm 1 and 732 cm 1 are due to Ti bondings. Impact Factor (JCC): Index Copernicus Value (ICV): 3.0

7 Synthesis and Characterization of Titanium Metal Carbon Nano Tubes 51 UV Visible Spectra Figure 4 increase. The spectra runs between 300nm 80nm for smaller size particles peaks become sharper and the absorbance h = Plank s constant C = Velocity of the light Energy of the band gap = h A Smaller gap means a larger energy absorption and hence shorter wavelength. The sample shows absorption at 410 nm. Figure 5 editor@tjprc.org

8 52 Uma Sharma & B. Tiwari CONCLUSIONS Titanium CNTs were synthesized with egg white proteins (albumin). The XRD and FTIR results, clearly confirmed the structures. The matrix base provided by egg white controls the size of the nanotube and gives it crystallinity.the heat treatment removes all organic volatile impurities and gives more purified sample in the crystalline form. The method is very cost effective which can be used for other materials. Water soluble egg white is environmental friendly also and controls the purity and size of the Titanium CNTs. REFERENCES 1. S. Chaturvedi, P. N. Dave, and N. K. Shah, Applications of nano-catalyst in new era, Journal of Saudi Chemical Society, vol. 16, no. 3, pp , View at Publisher View at Google Scholar View at Scopus 2. F. Cardarelli, Materials Handbook: A Concise Desktop Reference, 2nd edition, Z. Liu, Z. Jian, J. Fang, X. Xu, X. Zhu, and S. Wu, Low-temperature reverse microemulsion synthesis, characterization, and photocatalytic performance of nanocrystalline titanium dioxide, International Journal of Photoenergy, vol. 2012, Article ID , 8 pages, View at Publisher View at Google Scholar 4. X. Chen and S. S. Mao, Titanium dioxide nanomaterials: synthesis, properties, modifications and applications, Chemical Reviews, vol. 107, no. 7, pp , View at Publisher View at Google Scholar View at Scopus 5. M. Lal, V. Chhabra, P. Ayyub, and A. Maitra, Preparation and characterization of ultrafine TiO2 particles in reverse micelles by hydrolysis of titanium di-ethylhexyl sulfosuccinate, Journal of Materials Research, vol. 13, no. 5, pp , Impact Factor (JCC): Index Copernicus Value (ICV): 3.0