Micros

Inst.
Methods of Analysis 2/2/2011
Surface Characterization by
Microscopy
What are Electron

Microscopes?
• Electron Microscopes are scientific
instruments that use a beam of highly
energetic electrons to examine objects
on a very fine scale. The following
information can be obtained:
– Topography
• The surface features of an object or "how
it looks", its texture; direct relation
between these features and materials
properties (hardness, reflectivity...etc.)
Dr.Anandhan, MME, NITK 1

Inst.Methods of Analysis 2/2/2011
What are Electron

Microscopes?
– Morphology
• The shape and size of the particles making
up the object; direct relation between these
structures and materials properties
(ductility, strength, reactivity...etc.)
– Composition
• The elements and compounds that the
object is composed of and the relative
amounts of them; direct relationship
between composition and materials
properties (melting point, reactivity,
hardness...etc.)
What are Electron

Microscopes?
– Crystallographic Information
• How the atoms are arranged in the object;
direct relation between these arrangements
and materials properties (conductivity,
electrical properties, strength...etc.)

Specimen-beam
Specimen-
interactions
•Electrons incident on a material may

–scatter back
–knock out other (secondary) electrons
The number of secondary electrons produced is

relatively insensitive to atomic number of the atoms in
the material. The number of backscattered electrons,
however, is sensitive to atomic number of the material.

SEM - schematic
• Uses
– topographic images
– microstructural analysis
– elemental analysis if equipped with
appropriate detector (EDAX, WDX)
– magnification of 10 - 50,000
• Samples
– minimum size: 0.1 mm; maximum size
depends on machine
– samples must be conductive or coated with
thin conductive layer
– compatible with vacuum environment

SEM micrograph
x 500
Brittle fracture surface of steel
SEM micrograph
Vanadium oxide nanotubes

Transmission Electron
Microscope - schematic
Modes of operation
• Diffraction
– remove aperture
– look at diffracted beams from atomic planes
oriented to satisfy Bragg's Law
• Imaging
– insert aperture
– look at transmitted beam intensity

Anode
Glass Magnetic
coils
Under vacuum
TEM - operation
• Source of illumination is a filament
(cathode) that emits electrons at the top
of the column
– Since electrons are scattered by collisions
with air molecules, column must be under a
vacuum
• Electrons are accelerated by a nearby
anode
– Then passed through a tiny hole to form an
electron beam
• Magnetic coils focus the beam

TEM - applications
• Morphology
• Crystallographic Information
• Compositional Information (if so
equipped)
– The elements and compounds the sample is
composed of and their relative ratios, in
areas a few nanometers in diameter
TEM micrograph
Individual layers of clay are

seen in the micrograph
50 nm
Polymer-clay nanocomposite

TEM micrograph
Single-walled carbon nanotube
Atomic Force Microscopy

Atomic Force Microscope

(AFM)
• AFM stands for Atomic Force Microscopy
or Atomic Force Microscope and is often
called the "Eye of Nanotechnology".
• AFM, also referred to as SPM or
Scanning Probe Microscopy, is a high-
resolution imaging technique that can
resolve features as small as an atomic
lattice in the real space. It allows
researchers to observe and manipulate
molecular and atomic level features.
AFM - atomic force microscopy

A 'new' view of structure (1986)
CD stamper AlGaN/GaN quantum well waveguide
surface atoms on Si single crystal

See Vocabulary of Surface Crystallography,
polymer growth Journal of Applied Physics 35, 1306 (1964),
by Elizabeth A. Wood


How does the microscope work?
laser photodiode
diode
mirror
Tip scans sample
Up and down movement of tip

recorded by position sensing
photodiode
Si3N4
tip
sample


laser photodiode
diode
mirror
Tip scans sample
Up and down movement of tip

recorded by position sensing
photodiode
Si3N4
tip
sample

Two modes of operation laser photodiode

diode
mirror
Si3N4
tip
sample


Contact mode - short-range interactions (Å) - interatomic forces
Tip: 5-20 nm radius, 10-25 µm

high, on 50-400 µm
cantilever beam

Tip: 5-20 nm radius, 10-25 µm

high, on 50-400 µm
cantilever beam
Cantilever: low stiffness -

can't deform surface
Tip contacts surface
Tip scans surface: either tip or

specimen moved by
piezoelectric positioning
Detector system can measure system over x and y
deflections in nm range


Two ways - 'constant force' ……. feedback system

moves tip in z direction to keep force
constant
'constant height'……. no feedback system -

usually used when surface roughness small
higher scan speeds possible

Tapping mode - long-range forces - van der Waals,

electrostatic, magnetic
Tip vibrates (105 Hz) close to

specimen surface (50-150 Å)
with amplitude 10-100 nm
May at times lightly contact

surface
Suitable for soft materials


Tapping mode
Tip vibrates (105 Hz) close to

specimen surface (50-150 Å)
with amplitude 10-100 nm
May at times lightly contact

surface
When near or on surface,
Amplitude
oscillation is damped - tip z
position corrected so that
vibration amplitude stays
constant Tip height
From force-distance plot, can get:

range & magnitude of attractive & repulsive forces
elastic modulus & adhesion energy


Schematic of the contact mode AFM.

The normal and lateral forces, FN and FL , result in deflection and
torsion of the cantilever, respectively. They can be monitored using an
optical detection system and used for the purpose of feedback control
and/or image contrast formation.

Schematic of the intermittent contact mode AFM: free oscillation with free
amplitude Ao far away from sample surface, and damped oscillation with
set-point amplitude Asp and phase shift ∆Φ during scanning. Asp is chosen
by the operator, and feedback control is used to adjust tip-sample distance
such that Asp remains at constant value. The choice of Ao and Asp has great
influence on tip-sample force interaction and image formation.
Tip-
Tip-sample interaction


Phase image

3-D image of nanoparticles

Micros

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Inst.

Methods of Analysis 2/2/2011

What are Electron

Dr.Anandhan, MME, NITK 1

What are Electron

What are Electron

Dr.Anandhan, MME, NITK 2

•Electrons incident on a material may

The number of secondary electrons produced is

Dr.Anandhan, MME, NITK 3

Dr.Anandhan, MME, NITK 4

Brittle fracture surface of steel

Vanadium oxide nanotubes

Dr.Anandhan, MME, NITK 5

Dr.Anandhan, MME, NITK 6

Dr.Anandhan, MME, NITK 7

Individual layers of clay are

Dr.Anandhan, MME, NITK 8

Single-walled carbon nanotube

Atomic Force Microscopy

Dr.Anandhan, MME, NITK 9

Atomic Force Microscope

AFM - atomic force microscopy

CD stamper AlGaN/GaN quantum well waveguide

surface atoms on Si single crystal

Dr.Anandhan, MME, NITK 10

AFM - atomic force microscopy

Tip scans sample

Up and down movement of tip

Dr.Anandhan, MME, NITK 11

AFM - atomic force microscopy

Tip scans sample

Up and down movement of tip

AFM - atomic force microscopy

Two modes of operation laser photodiode

Dr.Anandhan, MME, NITK 12

AFM - atomic force microscopy

Contact mode - short-range interactions (Å) - interatomic forces

Tip: 5-20 nm radius, 10-25 µm

AFM - atomic force microscopy

Contact mode - short-range interactions (Å) - interatomic forces

Tip: 5-20 nm radius, 10-25 µm

Cantilever: low stiffness -

Tip contacts surface

Tip scans surface: either tip or

Dr.Anandhan, MME, NITK 13

AFM - atomic force microscopy

Contact mode - short-range interactions (Å) - interatomic forces

Two ways - 'constant force' ……. feedback system

'constant height'……. no feedback system -

AFM - atomic force microscopy

Tapping mode - long-range forces - van der Waals,

Tip vibrates (105 Hz) close to

May at times lightly contact

Suitable for soft materials

Dr.Anandhan, MME, NITK 14

AFM - atomic force microscopy

Tip vibrates (105 Hz) close to

May at times lightly contact

When near or on surface,

AFM - atomic force microscopy

From force-distance plot, can get:

Dr.Anandhan, MME, NITK 15