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Analysis of structural differences of Ag
Nanoparticles generated using
Thermal and E-beam process based
on SEM image
Presented by
Mainak Saha
Dept of Metallurgical and Materials Engineering
NIT Durgapur
Under guidance of
Dr. Shubhro Chakrabartty
Associate Professor, Dept. of ECE
Aurora’s Engineering College, Bhongir, Telangana
Introduction
• The variation in applications of nanoparticles comes from differences in their
microstructure.
• Nano range structures are formed by different methods.
• Lots of techniques are induced to develop nanoparticles such as chemical
process, RF sputtering, thermal evaporation, E-beam evaporation and etc
• Glancing angle deposition gives some special advantage of mechanism to create
nanostructures.
• The morphology of the nanostructures depends on rate of deposition, deposition
angle, substrate temperature and rotation rate.
Experimental procedure
• The GLAD technique has been carried out to synthesize the pure Ag (MTI,
USA) NPs on n-type Si <100> substrate.
• The substrates were rotated azimuthally with constant speed of 460 rpm
at an orientation of 85° with respect to the perpendicular line between
the metal source and the planar substrate holder.
• The depositions were carried out at a base pressure of ~2 × 10−5 mbar
inside the e-beam evaporator chamber. A deposition rate of 1.2 Å/s was
kept constant.
• The Ag NPs patterned was checked by FEG:SEM measurement.
Experimental procedure
• The depositions were carried out at a base pressure of ~2 × 10−5 mbar inside
the thermal evaporator chamber.
• The dimmestar voltage was 25 mV and time was 3 minutes to deposit the
particles over the substrate.
Equipment for Fabrication
Vacuum Chamber
Adjustable GLAD
TiO2 NWs/Si samples
DTM
Filament boat filled withAg
crystals
Path of Vapour
Clamps connected to current
supply
High Vacuum created by
Diffusion and Rotary Pump
Incident Vapour Flux
Rotating Substrate
Holder
α
ɸ
Angle of Rotation
Motor
Deposition angle
Thermal Evaporator cum GLAD apparatus
ThermalEvaporator
cumGLADsystem
Close view of E-beam evaporator
E-Beam Chamber
GLAD incorporated E-beam evaporator
Methodology
Flowchart
Feature calculated
• Length of the nano particles: Nanoparticles length was measured by
calculating the distance between two farthest point in the nanoparticle
boundary.
• Irregularity in a shape: Irregularity in the shape of each nanoparticles
derived by calculating the interior angles of the vertices of the detected
nanoparticles boundary.
• Area of the nano particles: The number of pixels inside a nanoparticle is
giving the area of the nano particles. The area was converted in nm unit
after multiplying with scaling factor.
Results and Discussion
• Average size is smaller for thermally generated nanoparticles than
nanoparticles generated using thermal and E-beam method.
• Irregularity is almost same for all of them.
• Low standard deviation for length and area of nanoparticles generated from
E-beam and thermal process proves the uniformity of nanoparticles.
• E-beam generated particles are more prominent.
Results and Discussion
Nanoparticle
Generation method
Length(nm) Area(nm2) Irregularity(o)
Mean
Standard
Deviation
Mean Standard
Deviation
Mean Standard
Deviation
Thermal 8.030 7.70 35.294 19.157 188.9443 6.02
E-beam 9.5564 3.5963 78.29 21.66 187.3196 6.5416
Results and Discussion
Nanoparticle
Generation
method
Length(nm) Area(nm2) Irregularity(o)
Thermal 31.68 148.8336 179.85
E-beam 27.28 411.2925 180
Microstructure of Ag NPs prepared by
Thermal Evaporation
Thermal cum GLAD
evaporator : Ag NPs
Maximum Demarcated NPs
All Demarcated NPs
(a) (b)
(c)
Microstructure of Ag NPs prepared by
E-beam evaporation
E-beam cum GLAD evaporator
: Ag NPs
Maximum Demarcated NPs
All Demarcated NPs
(a)
(b)
(c)
Conclusion
In conclusion we have done the comparative
morphological study of Ag nanoparticles
fabricated by E-beam evaporation method and
thermal evaporation method by Image
processing technique. The results project that
the particles grown by E-beam evaporator is
most prominent than Thermal evaporation
system.
Acknowledgement
Authors are thankful to the Council of Scientific
and Industrial Research (CSIR)-dt.11/05/2016
vide letter no. 03(1355)/16/EMR-II, National
Institute of Technology, Durgapur, West Bengal
and Dept. of Electronics and Communication
Engineering, National Institute of technology,
Agartala for using the laboratory and Aurora
Engineering college for the financial support.
References
• A. Vilchis-Nestor, V. Sánchez-Mendieta, M. Camacho-López, R. Gómez-Espinosa, M.
Camacho-López, J. Arenas-Alatorre, Solventless synthesis and optical properties of
Au and Ag nanoparticles using Camellia sinensis extractMater. Lett., 62 (2008), p.
3103
• Wan, Y., et al.: Quasi-spherical silver nanoparticles: Aqueous synthesis and size
control by the seed-mediated Lee-Meisel method. J. Colloid Interface Sci. 394,
263–268 (2013).
• P. Asanithi, S. Chaiyakun and P. Limsuwan, Growth of Silver Nanoparticles by DC
Magnetron Sputtering, Hindawi Publishing Corporation Journal of Nanomaterials
Volume 2012, Article ID 963609, 8 pages, 2012.
• A. Gurav, T. Kodas, L. Wang, E. Kauppinen J. Joutsensaari Chem. Generation of
nanometer-size fullerene particles via vapor condensation, Phys. Lett., 218 (1994),
p. 304
• F. Kruis, H. Fissan, B. Rellinghaus , Sintering and evaporation characteristics of gas-
phase synthesis of size-selected PbS nanoparticle , Mater. Sci. Eng. B, 69 (2000), p.
329
• Messier, R. Gehrke, T. Frankel, C. Venugopal, V. C. Otaño, W.and Lakhtakia, A.
(1997), Journal of Vacuum Science Technology. A, v.15, pp. 2148-2152.
• S. Chakrabartty, A. Mondal, M. B. Sarkar, B. Choudhuri, A. K. Saha, and A.
Bhattacharyya, “TiO2 Nanoparticles Arrays Ultraviolet-A Detector with Au Schottky
Contact” IEEE Photonics Technology Letters, Vol. 26, No. 11, 2014.
• N. Otsu, "A Threshold Selection Method from Gray-Level Histograms," IEEE
Transactions on Systems, Man, and Cybernetics, Vol. 9, No. 1, pp. 62-66, 1979.
• L. Di Stefano, A. Bulgarelli, A simple and efficient connected components labeling
algorithm, International Conference on Image Analysis and Processing, pp. 322-
327, 1999.
• Salembier, P., Oliveras, A. and Garrido, L., 1998. Antiextensive connected operators
for image and sequence processing. IEEE Transactions on Image Processing, 7(4),
pp.555-570.
• Araki, T., Ikeda, N., Molinari, F., Dey, N., Acharjee, S.M., Saba, L., Nicolaides, A. and
Suri, J.S., 2014. Effect of geometric-based coronary calcium volume as a feature
along with its shape-based attributes for cardiological risk prediction from low
contrast intravascular ultrasound. Journal of Medical Imaging and Health
Informatics, 4(2), pp.255-261.
THANK YOU

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Analysis of structural differences of Ag nanoparticles generated using Thermal and E-beam process based on SEM image

  • 1. Analysis of structural differences of Ag Nanoparticles generated using Thermal and E-beam process based on SEM image Presented by Mainak Saha Dept of Metallurgical and Materials Engineering NIT Durgapur Under guidance of Dr. Shubhro Chakrabartty Associate Professor, Dept. of ECE Aurora’s Engineering College, Bhongir, Telangana
  • 2. Introduction • The variation in applications of nanoparticles comes from differences in their microstructure. • Nano range structures are formed by different methods. • Lots of techniques are induced to develop nanoparticles such as chemical process, RF sputtering, thermal evaporation, E-beam evaporation and etc • Glancing angle deposition gives some special advantage of mechanism to create nanostructures. • The morphology of the nanostructures depends on rate of deposition, deposition angle, substrate temperature and rotation rate.
  • 3. Experimental procedure • The GLAD technique has been carried out to synthesize the pure Ag (MTI, USA) NPs on n-type Si <100> substrate. • The substrates were rotated azimuthally with constant speed of 460 rpm at an orientation of 85° with respect to the perpendicular line between the metal source and the planar substrate holder. • The depositions were carried out at a base pressure of ~2 × 10−5 mbar inside the e-beam evaporator chamber. A deposition rate of 1.2 Å/s was kept constant. • The Ag NPs patterned was checked by FEG:SEM measurement.
  • 4. Experimental procedure • The depositions were carried out at a base pressure of ~2 × 10−5 mbar inside the thermal evaporator chamber. • The dimmestar voltage was 25 mV and time was 3 minutes to deposit the particles over the substrate.
  • 5. Equipment for Fabrication Vacuum Chamber Adjustable GLAD TiO2 NWs/Si samples DTM Filament boat filled withAg crystals Path of Vapour Clamps connected to current supply High Vacuum created by Diffusion and Rotary Pump Incident Vapour Flux Rotating Substrate Holder α ɸ Angle of Rotation Motor Deposition angle Thermal Evaporator cum GLAD apparatus ThermalEvaporator cumGLADsystem
  • 6. Close view of E-beam evaporator E-Beam Chamber GLAD incorporated E-beam evaporator
  • 8. Feature calculated • Length of the nano particles: Nanoparticles length was measured by calculating the distance between two farthest point in the nanoparticle boundary. • Irregularity in a shape: Irregularity in the shape of each nanoparticles derived by calculating the interior angles of the vertices of the detected nanoparticles boundary. • Area of the nano particles: The number of pixels inside a nanoparticle is giving the area of the nano particles. The area was converted in nm unit after multiplying with scaling factor.
  • 9. Results and Discussion • Average size is smaller for thermally generated nanoparticles than nanoparticles generated using thermal and E-beam method. • Irregularity is almost same for all of them. • Low standard deviation for length and area of nanoparticles generated from E-beam and thermal process proves the uniformity of nanoparticles. • E-beam generated particles are more prominent.
  • 10. Results and Discussion Nanoparticle Generation method Length(nm) Area(nm2) Irregularity(o) Mean Standard Deviation Mean Standard Deviation Mean Standard Deviation Thermal 8.030 7.70 35.294 19.157 188.9443 6.02 E-beam 9.5564 3.5963 78.29 21.66 187.3196 6.5416
  • 11. Results and Discussion Nanoparticle Generation method Length(nm) Area(nm2) Irregularity(o) Thermal 31.68 148.8336 179.85 E-beam 27.28 411.2925 180
  • 12. Microstructure of Ag NPs prepared by Thermal Evaporation Thermal cum GLAD evaporator : Ag NPs Maximum Demarcated NPs All Demarcated NPs (a) (b) (c)
  • 13. Microstructure of Ag NPs prepared by E-beam evaporation E-beam cum GLAD evaporator : Ag NPs Maximum Demarcated NPs All Demarcated NPs (a) (b) (c)
  • 14. Conclusion In conclusion we have done the comparative morphological study of Ag nanoparticles fabricated by E-beam evaporation method and thermal evaporation method by Image processing technique. The results project that the particles grown by E-beam evaporator is most prominent than Thermal evaporation system.
  • 15. Acknowledgement Authors are thankful to the Council of Scientific and Industrial Research (CSIR)-dt.11/05/2016 vide letter no. 03(1355)/16/EMR-II, National Institute of Technology, Durgapur, West Bengal and Dept. of Electronics and Communication Engineering, National Institute of technology, Agartala for using the laboratory and Aurora Engineering college for the financial support.
  • 16. References • A. Vilchis-Nestor, V. Sánchez-Mendieta, M. Camacho-López, R. Gómez-Espinosa, M. Camacho-López, J. Arenas-Alatorre, Solventless synthesis and optical properties of Au and Ag nanoparticles using Camellia sinensis extractMater. Lett., 62 (2008), p. 3103 • Wan, Y., et al.: Quasi-spherical silver nanoparticles: Aqueous synthesis and size control by the seed-mediated Lee-Meisel method. J. Colloid Interface Sci. 394, 263–268 (2013). • P. Asanithi, S. Chaiyakun and P. Limsuwan, Growth of Silver Nanoparticles by DC Magnetron Sputtering, Hindawi Publishing Corporation Journal of Nanomaterials Volume 2012, Article ID 963609, 8 pages, 2012. • A. Gurav, T. Kodas, L. Wang, E. Kauppinen J. Joutsensaari Chem. Generation of nanometer-size fullerene particles via vapor condensation, Phys. Lett., 218 (1994), p. 304 • F. Kruis, H. Fissan, B. Rellinghaus , Sintering and evaporation characteristics of gas- phase synthesis of size-selected PbS nanoparticle , Mater. Sci. Eng. B, 69 (2000), p. 329 • Messier, R. Gehrke, T. Frankel, C. Venugopal, V. C. Otaño, W.and Lakhtakia, A. (1997), Journal of Vacuum Science Technology. A, v.15, pp. 2148-2152.
  • 17. • S. Chakrabartty, A. Mondal, M. B. Sarkar, B. Choudhuri, A. K. Saha, and A. Bhattacharyya, “TiO2 Nanoparticles Arrays Ultraviolet-A Detector with Au Schottky Contact” IEEE Photonics Technology Letters, Vol. 26, No. 11, 2014. • N. Otsu, "A Threshold Selection Method from Gray-Level Histograms," IEEE Transactions on Systems, Man, and Cybernetics, Vol. 9, No. 1, pp. 62-66, 1979. • L. Di Stefano, A. Bulgarelli, A simple and efficient connected components labeling algorithm, International Conference on Image Analysis and Processing, pp. 322- 327, 1999. • Salembier, P., Oliveras, A. and Garrido, L., 1998. Antiextensive connected operators for image and sequence processing. IEEE Transactions on Image Processing, 7(4), pp.555-570. • Araki, T., Ikeda, N., Molinari, F., Dey, N., Acharjee, S.M., Saba, L., Nicolaides, A. and Suri, J.S., 2014. Effect of geometric-based coronary calcium volume as a feature along with its shape-based attributes for cardiological risk prediction from low contrast intravascular ultrasound. Journal of Medical Imaging and Health Informatics, 4(2), pp.255-261.