www.seattlenano.

org

Nanotechnology
Characterization
SHINE: Seattle’s Hub for Industry-driven Nanotechnology Education
North Seattle College
Characterization Techniques

Two types of nanomaterial characterization:

• Spectroscopic methods
• i.e. UV-VIS, DLS
• Imaging methods
• i.e. TEM, SEM, AFM

Source: NSC students Source: NSC students

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0-D Nanoparticles

Color of a nanoparticle solution is dependent on

nanoparticle size.

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UV-Vis Absorption

Gives quantitative measure of color.

What wavelengths are absorbed?
What wavelengths are transmitted?

Source: Cytodiagnostics

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UV-Vis Spectrometer

Source: Vernier

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Dynamic Light Scattering (DLS)

DLS measures the Brownian motion of the nanoparticles

and correlates this to particle size

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Dynamic Light Scattering (DLS)

DLS instrument

Source: www.Malvern.com

Source: NSC Students

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Imaging Methods

Light (Optical) Microscopy SEM micrograph

Electron Microscopy
• TEM
• SEM
Scanning Probe Microscopy
• STM
• AFM
• Profilometry

Source: NSC Students

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Resolution Limit

Light microscopes
• 500 X to 1500 X magnification
• Resolution of ~0.2 µm
• Limits reached by early 1930’s

Resolution dependent on:

• wavelength of illumination () 0.612
d
• Numerical Aperture (NA) of lens system NA

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Electron Microscopes

Wavelength of the electron dependent on:

• Electron mass (m)
• Electron charge (q)
• Potential difference to accelerate electrons (V)

h

2mqV
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Transmission Electron Microscope

Transmission Electron Microscope

(TEM)
1. e-beam strikes sample
and is transmitted through
the sample
2. Scattering occurs
3. Un-scattered electrons
pass through sample and
are detected

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Transmission Electron Microscope
TEM
Copper Grid Sample Holder

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TEM Images
Inorganic Material

Organic Material

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Scanning Electron Microscope

Scanning Electron Microscope (SEM)

1. e- beam strikes sample and
electron penetrate surface
2. Interactions occur between
electrons and sample
3. Electrons and photons
emitted from sample
4. Emitted e- or photons
detected

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Scanning Electron Microscope (SEM)

SEM Conidia of Aspergillus

Aspex Explorer located at NSC

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Scanning Electron Microscope (SEM)

SiO2 spheres A succulent plant

Source: NSC Students Source: NSC students

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Scanning Electron Microscope (SEM)

A hair “split end” A “bug” eye

Source: NSC Students Source: NSC students

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Scanning Probe Microscopy

Measure feedback from atomically defined tip

Many types of feedback (dependent on tip)

AFM – Forces between sample and tip

STM – Tunneling current between sample and tip

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Scanning Tunneling Microscope
• Tip scans just above
surface of stage
• Electrons have a small
probability of escaping
material to tip creating
tunneling current
• Tunneling current is
depends on distance
between tip and
sample
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STM Images
• “See” individual atoms
• Must have high vacuum , low temp (4 K)

Pt and Ni atoms on an alloy surface STM at University of Wisconsin –

Eau Claire

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Atomic Force Microscope (AFM)

1. Tip scans across surface

2. Laser reflects off of
cantilever to a
photodetector
3. Feedback loop changes
tip to sample distance
4. Height changes recorded

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Atomic Force Microscopy (AFM)
AFM Cantilevers and tips

Source: NSC Students Source: NSC Students Source: NSC Students

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Atomic Force Microscopy (AFM)
Nanosurf EasyScan 2

Source: NSC
Students
Source: SHINE

Butterfly Wing

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Profilometery
0.5 nm resolution in the Z-direction

Bruker Dektak XT profilometer Typical profilometer scan

Source: NSC students

Source: NSC students

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3-D Profilometery

2-D profilometer scan 3-D profilometer scan

Source: NSC students

Source: NSC students

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Image References
Slide 3 Adv. Mater. 2006., 18, 2529 - 2534

Gold nanoparticle shape dependent LSPR. Cytodiagnostics. [Online Image]. 8

Slide 4 May 2016. <http://www.cytodiagnostics.com/store/pc/Introduction-to-Gold-
Nanoparticle-Characterization-d3.htm>

SpectraVis Plus Spectrophotometer. Vernier. [Online Image]. 8 May 2016.

<http://www.vernier.com/products/sensors/spectrometers/visible-range/svis-
pl/>
Slide 5 Spectrometer Diagrams. Adapted from Hewlett-Packard's "Fundamentals of
Modern UV-Visible Spectroscopy" publication number 12-5965-512E, 1996.
[Online Image]. 8 May 2016 <http://www.the-
scientist.com/?articles.view/articleNo/18797/title/Across-the-Spectrum--
Instrumentation-for-UV-Vis-Spectrophotometry/>

Dynamic Light Scattering. Jones, Mike. [Online Image]. 21 June 2016.

Slide 6
<https://commons.wikimedia.org/wiki/File:DLS.svg>

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Image References
Intensity Fluctuations and Brownian Motion. AZO Materials. [Online Image] 10
May 2016. <http://www.azom.com/article.aspx?ArticleID=12255>
Slide 6 Weighted Distributions. Yilun LiAndrew R. Barron, Dynamic Light Scattering.
OpenStax CNX. May 7, 2014 http://cnx.org/contents/3fc98dad-934d-45e6-
a19f-c0a1cf440d43@1.>

Microscope. [Online Image] 10 May 2016.

Slide 7
<http://mssmith.wicomico.wikispaces.net/Tools+Scientists+Use>

Transmission Electron Microscope. Wikimedia Commons. [Online Image]. 10

Slide 11 May 2016
<https://commons.wikimedia.org/wiki/File:Electron_Microscope.png>

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Image References
TEM. Boundless. “Electron Microscopy.” Boundless Microbiology. Boundless,
13 Apr. 2016. Retrieved 10 May. 2016 from
<https://www.boundless.com/microbiology/textbooks/boundless-microbiology-
textbook/microscopy-3/other-types-of-microscopy-30/electron-microscopy-249-
Slide 12 1065/>
3 mm copper grid. Lilly_M. Wikimedia Commons. [Online Image]. 17 May 2016.
<https://commons.wikimedia.org/wiki/File:3_mm_copper_grid_electron_micro
scopy_for_sample-04.jpg>

Golgi Apparatus. [Online Image]. 17 May 2016.

<https://courses.candelalearning.com/biology11xmaster/chapter/eukaryotic-
Slide 13 cells/>
Mesoporous silica nanoparticle. [Online Image]. 21 May 2016.
<https://en.wikipedia.org/wiki/File:Mesopourus_silica_closeup.jpg>

SEM Image. MyScope. [Online Image]. 21 May 2016. <http://li155-

Slide 14
94.members.linode.com/myscope/sem/practice/principles/layout.php>

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Image References
Conidium. Gans, Murray. [Online Image]. 21 May 2016. <http://murry-
Slide 15 gans.blogspot.com/2013_04_01_archive.html>

Scanning Tunneling Microscope. [Online Image]. 22 May 2016.

Slide 19 <https://en.wikipedia.org/wiki/Scanning_tunneling_microscope#/media/File:
ScanningTunnelingMicroscope_schematic.png>

Pt and Ni. Richmond, Michael. [Online Image]. 22 May 2016.

<http://spiff.rit.edu/classes/phys314/lectures/stm/stm.html>
Slide 20
STM. [Online Image]. 22 May 2016.
<http://www.uwec.edu/Matsci/center/instrumentation/>

AFM. Hansma, Helen. [Online Image]. 22 May 2016.

Slide 21 <http://web.physics.ucsb.edu/~hhansma/biomolecules.htm>

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Image References
Butterfly Wing. NanoSurf. [Online Image]. 22 May 2016.
Slide 22 <https://www.nanosurf.com/en/application/70-butterfly-wings-a-fragile-
biological-nanostructure>

To access additional educational resources

please visit: www.seattlenano.org

This material is based upon work supported by the National Science Foundation under Grant Number
1204279. Any opinions, findings, and conclusions or recommendations expressed in this material are
those of the author(s) and do not necessarily reflect the views of the National Science Foundation.

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