MSO-326(a)

Nanomaterials & Technology

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 Advantages_PVD
 Materials can be deposited with improved properties
compared to the substrate material

 Almost any type of inorganic material can be used

as well as some kinds of organic materials

 The process is more environmentally friendly than

processes such as electroplating.

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 DISADVANTAGES
 It is a line of sight technique meaning that it is
extremely difficult to coat undercuts and similar
surface features
 High capital cost
 Some processes operate at high vacuums and
temperatures requiring skilled operators
 Processes requiring large amounts of heat require
appropriate cooling systems
 The rate of coating deposition is usually quite slow
DIFFERENCE BETWEEN PVD AND CVD

PVD uses Physical Processes While CVD Primarily uses

only Chemical processes

PVD typically uses a Pure source while CVD uses a Mixed

material source material

http://www.hindawi.com/journals/jnm/2012/486301.fig.002.jpg
 FACTORS THAT AFFECT DEPOSITION OF THIN
FILMS

1 . Substrate surface condition before and after cleaning and

surface modification such as surface morphology (roughness,
inclusions, particulate contamination), surface chemistry (surface
composition, contaminants), mechanical properties, surface
flaws, out gassing, preferential nucleation sites, and the stability
of the surface.

2. Details of the deposition process and system geometry such

as deposition process used, angle-of-incidence, distribution of the
depositing adatom flux, substrate temperature, deposition rate,
gaseous contamination, concurrent energetic particle
bombardment (flux, particle mass, energy).
3.Post deposition processing and reactions such as chemical
reaction of the film surface with the ambient, subsequent
processing, thermal or mechanical cycling, corrosion,
interfacial degradation; surface treatments such as burnishing of
soft surfaces, overcoating ("topcoat"), or chemical modification
such as chromate conversion.
Characterization of nanomaterials
 Fundamentals of SEM: imaging
modes, image contrast, illustrative
applications

(Microstructural Analysis)
Short history of SEM (Scanning electron
microscopy)
 1897: e discovered by J.J. Thompson (Noble
prize 1906)
 1924: Wave particle dualism postulated by de
Broglie (Noble prize 1929)
• TEM constructed in 1931
• Von Ardenne first STEM in 1938 by rastering the
electron beam in a TEM
• Zworykin et al. 1942, first SEM for bulk samples
• 1965 first commercial SEM by Cambridge Scientific
Instruments
Interaction of Electron Beam with Matter
 Continuous improvement in the
technology

Resolution at that time ~ 50 nm <-> Today < 1 nm

Morphology only at that time <-> Today analytical instrument

Energy distribution of BSE and SE
electron
Schematic of SEM
• Electron Gun
• EM Lens
• Specimen
Chamber/Stage
• Scanning
• CRT/ Display
• Vacuum System

SEP ppt by Anders Werner Bredvei Skilbred; Harald Fjeld

 How do we get an image?
Electron gun
156
288 electrons!
electrons!

Detector

Image

MENA3100
SEM Operation
 Scanning Electron Microscopy
• Imaging of features as small as 10 nm or less, roughly 100
times smaller than can be seen with light microscopes
• Imaging of rough surfaces
• Qualitative and semi-quantitative elemental analysis on
microstructural features as small as 2 µm
• Identifying crystalline compounds and determining
crystallographic orientations of microstructural features
as small as 1 µm (recently developed capability--not
currently widely used, but likely to become so)
 SEM parameters

• Mlinear = Size of the display/Size of the scanned area

• Resolution:
– Resolution can not be better than the e-beam size
– Typically limited by the lateral dimension of the interaction
volume
 Electron beam-sample interactions
• The incident electron beam is scattered in the sample, both
elastically and inelastically
• This gives rise to various signals that we can detect (more on
that on next slide)
• Interaction volume increases with increasing acceleration
voltage and decreases with increasing atomic number

Images: Smith College Northampton, Massachusetts

 Where does the signals come from?

• Diameter of the interaction

volume is larger than the electron
spot
 resolution is poorer than the
size of the electron spot

Image: Department of Geology and

Geophysics, Louisiana State University
MENA3100
 Summary
• Signals:
– Secondary electrons (SE): mainly
topography
• Low energy electrons, high resolution
• Surface signal dependent on curvature
– Backscattered electrons (BSE): mainly
chemistry
• High energy electrons
• “Bulk” signal dependent on atomic number
– X-rays: chemistry
• Longer recording times are needed
Secondary/Backscattered Electrons
S. No. Secondary Backscattered

Scattering Inelastic Elastic

Depth ~10 nm 0.5-1 µm

Energy < 50 eV > 50 eV (generally

similar to that of
incident beam)

Topographic Contrast Yes Yes

Compositional No Yes

Resolution Finer Coarser

 Applications
• Characterizing fractured surface: dimple, cleavage,
fatigue, etc.
• Quality assurance examination of microelectronic
devices, interconnections, bonds, etc.
• Detecting the onset of corrosion in small components
• Resolving fine microstructural features
• Performing qualitative and semi-quantitative
elemental analyses (Using EDS/WDS attachment)
• Characterizing preferred crystallographic orientations
by analysis of orientations of individual grains
 Images

Optical SEM
 W-filament

LaB6 filament Field Emission Gun

 Ductile Fracture

http://www.metalworking.com/Dropbox/BrokenD
eckelStud1.jpg
http://www.eatechnology.com/content/uploaded/images/9
6a84d05-7e89-4270-bad0-d289f0e6968f.jpg
 Brittle Fracture

http://met-tech.com/images/fractured-input-shaft-7.jpg http://www.unl.edu/CMRAcfem/gifs/fracture.jpg
 Ni in Al2O3 matrix

• Details
• Composition