caracterizaÇÃo de nanoparticulas e nanoestruturas aula 10 qf933 instituto de química unicamp
DESCRIPTION
CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP. Nanoparticles Characterization: Measurement of the particles size by the PCS technique. MSc. Priscyla D. Marcato Dr. Nelson Durán. Principle of Measurement. - PowerPoint PPT PresentationTRANSCRIPT
![Page 1: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/1.jpg)
CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS
Aula 10 QF933Instituto de Química
UNICAMP
![Page 2: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/2.jpg)
Nanoparticles Characterization:Nanoparticles Characterization:
Measurement of the particles Measurement of the particles size by the PCS techniquesize by the PCS technique
MSc. Priscyla D. MarcatoDr. Nelson Durán
![Page 3: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/3.jpg)
• If the particles or molecules are illuminated with a laser, the intensity of the scattered light fluctuates at a rate that is dependent upon the size of the particles
• Analysis of these intensity fluctuations yields the velocity of the Brownian motion and hence the particle size using the Stokes-Einstein relationship.
Principle of Measurement
![Page 4: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/4.jpg)
Brownian Motion
Particles, emulsions and molecules in suspension undergo
Brownian motion.
This is the motion induced by the bombardment by solvent
molecules that themselves are moving due to their thermal
energy
Temperature and viscosity must be known
![Page 5: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/5.jpg)
Intensity of the scattered light fluctuates
![Page 6: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/6.jpg)
Intensity of the scattered light fluctuates
Small particles- noisy curve
Large particles- smooth curve
![Page 7: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/7.jpg)
The velocity of the Brownian motion is defined by a property known as the translational diffusion coefficient (usually given the symbol, D).
Stokes-Einstein relationship
![Page 8: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/8.jpg)
![Page 9: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/9.jpg)
Zetasizer Nano ZS Malvern
He-Ne Laser = 633 nm
![Page 10: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/10.jpg)
Determining particle size
Determined autocorrelation function
Depend
![Page 11: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/11.jpg)
Correlation function Correlograms
![Page 12: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/12.jpg)
Correlogram from a sample containing
large particles
Correlogram from a sample containing
small particles
![Page 13: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/13.jpg)
![Page 14: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/14.jpg)
![Page 15: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/15.jpg)
![Page 16: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/16.jpg)
Lowconcentration turbidity is linear with
concentration
High concentration
Particles are so close together that the scattered radiation is re-scattered by other particles.
![Page 17: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/17.jpg)
Optical arrangement
in 173°
backscatter detection
![Page 18: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/18.jpg)
Information
Size by:
- Intensity I d6
Rayleigh Scattering(For nanoparticles less than d =λ/10 or around 60nm
the scattering will be equal in allDirections-isotropic)
![Page 19: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/19.jpg)
This particles will scatter 106 (one million) times more light than the small particle (8 nm)
The contribution to the total light scattered by the small particles will be extremely small
8 nm80 nm
![Page 20: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/20.jpg)
8 80
![Page 21: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/21.jpg)
- Volume d3
d1- Number
V= 4r3 r = d/2V= 4(d/2)3 = 4d3
8
By the Mie theory is possible convert intensity distribution into volume
![Page 22: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/22.jpg)
Two population of spherical nanoparticles : 5 nm and 50 nm
(in equal number)
Which of these distributions should I use?
![Page 23: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/23.jpg)
d(intensity) > d(volume) > d(number)
![Page 24: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/24.jpg)
![Page 25: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/25.jpg)
![Page 26: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/26.jpg)
![Page 27: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/27.jpg)
Direct determination of the number-weighted mean radius and polydispersity from dynamic light-scattering dataPhilipus et al., Applied Optics, 45, 2209 (2006)
We find that converting intensity-weighted distributions is not always reliable, especially when the polydispersity of the sample is large.
![Page 28: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/28.jpg)
![Page 29: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/29.jpg)
![Page 30: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/30.jpg)
Reference
Dynamic Light Scattering:An Introduction in 30 Minutes, Malvern, http://www.malvern.co.uk/common/downloads/campaign/MRK656-01.pdf
![Page 31: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/31.jpg)
HOMOGENEIZAÇÃO À ALTA PRESSÃO
![Page 32: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/32.jpg)
Solução de tensoativo (quente)
(sob alta agitação)
Homogeneizado à alta Pressão
Ativo + Lipídio fundido
Moído (micropartículas lipídicas)
Micro-suspensão
Solução de tensoativo (fria)
AgitaçãoAgitação
Pré-emulsão
Homogeneização a quente
Solidificação(nitrogênio líquido)
Homogeneização a frio
![Page 33: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/33.jpg)
![Page 34: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/34.jpg)
• Rápido e Fácil
•Fácil escalonamento - 99% de reprodutibilidade em escala
industrial
• Evita contaminação no processo de homogeneização
Homogeneização à Alta Pressão
![Page 35: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/35.jpg)
Espectroscopia de Correlação de Fótons
![Page 36: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/36.jpg)
Espectroscopia de Correlação de Fótons
Diâmetro
![Page 37: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/37.jpg)
Potencial Zeta
Espectroscopia de Correlação de Fótons
![Page 38: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/38.jpg)
• Rápido e Fácil
•Fácil escalonamento - 99% de reprodutibilidade em escala
industrial
• Evita contaminação no processo de homogeneização
![Page 39: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/39.jpg)
Dingler e Gohla, J.Microencapsul.19, 11-16 (2002).
![Page 40: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/40.jpg)
500 bar 3 ciclos
Sakulkhul et al., Proceedings of the 2nd IEEE International ( 2007)
![Page 42: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/42.jpg)
![Page 43: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/43.jpg)
![Page 44: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/44.jpg)
![Page 45: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/45.jpg)
![Page 46: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/46.jpg)
![Page 47: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/47.jpg)
![Page 48: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/48.jpg)
![Page 49: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/49.jpg)
![Page 50: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/50.jpg)
![Page 51: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/51.jpg)
![Page 52: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/52.jpg)
![Page 53: CARACTERIZAÇÃO DE NANOPARTICULAS E NANOESTRUTURAS Aula 10 QF933 Instituto de Química UNICAMP](https://reader035.vdocuments.mx/reader035/viewer/2022070423/568167de550346895ddd3c0f/html5/thumbnails/53.jpg)