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E.G.S.

PILLAY ENGINEERING COLLEGE

SYNTHESIS AND CHARACTERIZATION OF NANO SILICON CARBIDE PARTICLES (NANO SICP)


PROJECT GUIDE
MR. S. KRISHNA MOHAN, M.E., (PH.D.,) ASSOSIATE PROFESSOR DEPARTMENT OF MECHANICAL

BATCH MEMBERS
MR. K.AYYAPPAN (80608144005) MR. K.MANI KANDAN (80608144021) MR. M.MOHAMED THAMIMUL ANSARI (80608144025) MR. B.PRASANTH (80608144033)

LITERATURE SURVEY
Morphological And Optical Characterization Of Porous Silicon Carbide F. Hassen (a), R. M Ghaieth (a), H. Maaref (a), R. Mader (b).

A Study On The Effect Of Silica Particle Size And Milling Time On Synthesis Of Silicon Carbide Nano Particle By Carbothermic Reduction B.M. Moshtaghioum , A. Monshi, M.H. Abbasi, F. Karimzadeh Comminution Of Silicon Carbide Powder In Planetary Mill Maria Aparcida P. dos Santos (a), Celio A. Costa (b)
Some Studies On Synthesis Of Nano SiCp S. Krishna Mohan (a), Dr. S. Ramanathan (b) Synthesis And Characterization Of 356-Sicp Composites By Stir Casting And Compo casting Methods S. Amirkhanlou, b. Niroumand

LITERATURE SURVEY
Micro structural characterization of -SiC powders synthesized by carbothermally reduction of Turkish diatomite Cengiz Bagci Materials Processes of Graphite Nanostructure Composites Using Ball Milling Shing-Chung Wong1, Eric M. Sutherland2, and Fawn M. Uhl3

Synthesis of Silicon Carbide by Reaction Milling in a Dual-drive Planetary Mill Debasis Chaira, B. K. Mishra, S. Sangal
Synthesis and characterization of 356-SiCp composites by stir casting and compocasting methods. Amirkhanlou, b. Niroumand Processing And Characterization Of Silicon Carbide Sang-Kwon Lee

ABSTRACT
Silicon carbide (SiCp) is a very interesting ceramic due to its promising properties like high hardness, high strength, low bulk density, good wear and corrosion resistance, high oxidation resistance which makes it useful for a wide range of industrial application are abrasives, cutting tools, heating elements, thermal barriers for aeronautics or aerospace applications. Silicon carbide based semi conductors, electronic devices and circuits are presently developed for use in high temperature, high power and high radiation conditions. There are several methods are available to produce Nano materials such as form In phase, mechanical method, case phase synthesis and wet chemistry. In this study we Adopt Mechanical topdown method that reduce the size of particles by ball milling or planetary milling. After preparation of nano particles, this will be characterized by AFM, particle analyzer ,SEM and comparison of different nano SiCp..

WORK PROCESS CHART


Raw SiCp characterization
Synthesis by planetary milling

Nano SiCp

Characterization of nano SiCp

AFM

SEM

Particle analyze

Conclusion

RAW SILICON CARBIDE POWDER

Grain size of raw silicon carbide is 30 microns

PLANETARY MILLING (OR) BALL MILLING


A ball mill, a type of grinder, is a cylindrical device used in grinding (or mixing) materials like ores, chemicals, ceramic raw materials and paints

Specification of ball milling


Maximum sample quantity :225 ml No. of balls :50 and 100 (tungsten) Materials of the grinding tools: tungsten Running time :8&5hrs(per sample 20 grams) pause time :5 min Grinding process :dry/wet speed :300 rpm Bp ratio :20:1 and 40:1

PLANETARY MILLING PROCEDURE

Two samples were prepared with respect to milling time and Bp ratio. Sample 1 prepared 8 hrs and BP ratio 20:1 Sample 2 prepared 5hr and Bp ratio 40:1 Fed the 20 grams sic powder

NANO SILICON CARBIDE PARTICLE

SAMPLE PREPARATION
The milled nano SiC powder were mixed with acetone solution and treated in ultrasonic sonicator (750 W,20 kHz, sonic-USA) for about 10 minutes to attain individual particles from agglomeration. Using drop cast approach, few drops of suspension prepared from sonicator is deposited on the plain glass plate and allowed for 10 minute for drying then characterized.

Ultrasonic sonicator

AFM (ATOMIC FORCE MICROSCOPE)

Atomic force microscopy (AFM) is a technique for analyzing the surface of a rigid material all the way down to the level of the atom . AFM uses a mechanical probe to magnify surface features up to 100,000,000 times, and it produces 3-D images of the surface..

AFM INSTRUMENT

(AFM) (XE 70, Park System- Korea)

SAMPLE 1
SURFACE MORPHOLOGY

The AFM images shows the surface features or morphology of the Raw SiC and sample in microns X micron size images. The AFM images were taken in vertical and horizontal line scans. Those line scans reveal the depth profile. the red color right scan says the profile from the top (2.5) to the bottom (-2.5) totally 5 nm depth. the same results absorbed in the left image also. it is observed that the height of cone like shape vertically from the surface (fig.2). comprehensively the surface topology on AFM at height and depth in nano scale was observed.

SAMPLE 2

The AFM images shows the surface features or morphology of the Raw SiC and sample in microns X micron size images. The AFM images were taken in vertical and horizontal line scans. Those line scans reveal the depth profile. the red color right scan says the profile from the top (2.5) to the bottom (-2.5) totally 5 nm depth. the same results absorbed in the left image also. it is observed that the height of cone like shape vertically from the surface (fig.2). comprehensively the surface topology on AFM at height and depth in nano scale was observed.

PARTICLE ANALYSIS (ZETA SIZER)

The Zeta sizer Nano range of instruments provides the ability to measure three characteristic of particles or molecules in a liquid medium. These three fundamental parameters are Particle size, Zeta potential and Molecular weight

ZETASIZER EQUIPMENT:

SAMPLE 1

Table 1 (Size Statistics Report by intensity)

Table 2 (Size Distribution Report by intensity)

CONTEND
The Statistics Report by intensity (table 1&2) shows the average particle size of SiCp nano particle and the things always will be a Gaussian distribution mean will be a peak in a border way thats what got in fig. the peak start at 100 nm and end at 1000 nm and again starts from there and ends at 10000 nm. This says that we have particles from 100 nm to 10000 nm, but 100-10000 nm is more. The peak center is around 500 nm which says that the average particle size is around 500 nm; the exact value is shown in the peak value as 432.9 nm.

SAMPLE 2

Table 1 (Size Statistics Report by intensity)

Table 2 (Size Distribution Report by intensity)

CONTEND
The Statistics Report by intensity (table 1&2) shows the average particle size of SiCp nano particle and the things always will be a Gaussian distribution mean will be a peak in a border way thats what got in fig. the peak start at 100 nm and end at 1000 nm and again starts from there and ends at 10000 nm. This says that we have particles from 100 nm to 10000 nm, but 100-10000 nm is more. The peak center is around 500 nm which says that the average particle size is around 500 nm; the exact value is shown in the peak value as 315.5 nm.

Work in progress
SEM (SCANNING ELECTRON MICROSCOPE) A scanning electron microscope (SEM) is a type of electron microscope that images a sample by scanning it with a high-energy beam of electrons in a raster scan pattern. The electrons interact with the atoms that make up the sample producing signals that contain information about the sample's surface topography, composition, and other properties such as electrical conductivity.

WORKING OF SEM

SEM IMAGES
RAW SiCp

SAMPLE 1

SAMPLE 2

CONTEND
The SEM technique was used to follow the changes in shape and size of the milled powders during the different stages of the reaction milling process. the SEM micrographs of the milled powders after different intervals of milling time. In all the micrographs the marker is

set at micron. At the initial stages of milling, the powders of the Raw
SiCp are bulky, with random shape and size. As the milling progressed the powders became very small size which correspond to hours of

milling and Bp ratio. It is also evident from the SEM images that it
decreases gradually particle size with increasing milling time and Bp ratio.

CONCLUSION
SiC

can be synthesized through high-energy reaction milling at room temperature There is an effect of ball size on reaction milling. The amount of impact increases with increasing ball diameter. As the milling time increases, powder particles become finer and contain more defects

BIBLIOGRAPHY
www.material science.com www.paletarymilling.com www.nanonics.com www.elsevier.com www.webminerals.com www.particle-analytical.com www.directscience.com

COST ESTIMATION
Serial. no 1 2 3 5 6 description Planetary milling AFM SEM Particle analysis total amount 5000 2500 3000 2000 12500

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