Optical and Atomic Force microscopies

Morphological characterization of
surface and objects from micronic down
to atomic scale
Dr. Florence Marchi
florence.marchi@neel.cnrs.fr
http://neel.cnrs.fr/
Aim of the whole course (Nano I and Nano II):
To underline the pluri-disciplinary aspects in Nanosciences
research, a crosstalk in physic, chemistry and biology at
nanoscale.

Aim of this course part of Nano I :

To introduce optical and scanning force microscopies (SFM);
SFM are powerful techniques to observe and to study
objects at micro and nanoscales 1
 Néel Institute - Grenoble Université Alpes
Ø Fundamental research in physics of condenser matter enriched
by interdisciplinary activities at the interfaces with chemistry,
engineering and biology.
Ø Establishment in 2007 through three departments, 17
research teams and 17 technical groups • 1940 Louis Néel settled to
§ PLUM: Physique LUmière Matière Grenoble
§ QUantum Electronics , Surfaces and spinTronics (QUEST) • 1946 : inauguration of the
§ Condensed Matter - Low Temperatures (MCBT) 1st CNRS Lab outside Paris!

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 Content of Optical and Scanning force microscopy course (8h in total)
• Fours courses (4*2h=8h) : 10/01AM; and 12/01AM, 12/01PM ; 17/01 AM
• Definitions of Nanosciences & Nanotechnologies, nano-object
• Specificity of sub-micronic objects
• Forces acting at nanoscale
• Characterization techniques of (sub)micronic and nanometric object in the
direct space
• Optical microscopies
• Basic concepts of a classical optical microscope
• Diffraction limit
• Far-field optical Nanoscopy for nanoscale visualization
• Atomic Force microscopy
• General Principle and image formation
• Static or dynamic mode ?
• AFM in liquid : what are the main differences with working in air ?
• Resolution of the technique
• How to probe mechanical response of an object at nanoscale ?
• Image processing

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 General information and Schedule of Practical Works 2024 related to AFM

• 1st PW : Introduction to AFM (4h): on the Nanoworld platform located at CIME:

Dates (Fiday) :; 19th; 26th of January and 02th of February
Time slots : 8:00am-12:00am or 1:30pm-5:30pm
PW related to Nanosciences 1

• 2nd PW : Combined Nanobiophysic PW : CUBE and Nanoworld Platforms

• 1st slot on CUBE platform (7h) : in March with Pr. E Planus (IAB) & Dr V.
Stoppin-Mellet (GIN)
• 2nd slot on the Nanoworld platform (4h) with Dr. E Planus or Dr V. Stoppin-
Mellet and Dr. F. Marchi
Dates : End of March and Beginning of April (according to your
group number)
Time slots : 8:00am-12:00am or 1:30pm-5:30pm
PW related to Nanosciences 2

• UE Evaluation : After each PW a report has to be written and send to the teacher(s)
for evaluation. An final exam will take place at the end of the semester.
The global mark of this UE is a balance between the mark related to the PW reports
evaluation and the final exam. 4
 How to come and access to CIME Nanotech ?
University area in MINATEC campus
https://cime.grenoble-inp.fr/

Tram B, “Cité Internationale” station, CIME is located inside G-INP

Minatec campus. 5
 Definitions and basics review
• Classification of object scale

• What is called a ‘nano-object’ or a ‘Nano-materials”?

• Some examples of nanotechnology fields

• Specific properties at nanoscale

» Ratio: Volume/Surface
» Quantum effects and surface interactions

• Optical microscopy to observe down to microscale: principle and limitations

• Scanning Force Microscope to observe and measure beyond the (sub)micronic scale

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 « Definitions » related to Nanociences and Nanotechnologies

q Scale review: 1nm = 10-9m = 0.001µm

q Nano-object&Nanomaterials: An object of which at least one dimension is

about less that few hundreds of nanometers
q Nanosciences: ‘Hard’ sciences perform at nanoscale to study the
chemical, physical and/or biological properties

q Nanotechnologies:
ü Technological capabilities required to fabricate nano-objects and nano-
devices
ü To apply the specific properties of matter and its associated interactions
to develop and fabricate original devices at nanoscale..

q Exercise : Could you classify from the larger to the smaller these objects ?
ü Diameter of DNA strand ü Hair diameter
ü Visible light ü Virus
ü Carbon nanotube diameter ü Red cell
ü Atom diameter ü Graphene layer thickness
ü Bacteria ü Nanoparticles
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 Examples of Biological objects and particles

https://abcdust.net/quelle-est-la-taille-dun-virion-covid-19-par-
rapport-au-mp10-25/?lang=fr

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Examples of Nano-object&Nanomaterials

The Graphene :
The « Star » of the 2D materials
• Young’s modulus (stiffness) close to 1 TPa,
same as Diamond
• At RT, the resistivity of graphene sheets is
about 10−8 Ω⋅m. This is less than the
resistivity of silver (1,59×10 −8) .

https://en.wikipedia.org/wiki/File:Graphene_
and_Dirac_Cones.ogv 9
 m
Radius size 116p
O
C
O
Molecule

ELECTRON

ATOM NUCLEUS QUARK

Amstrom (Å)
PROTONS
Femtometer (fm)
attometre
(am)

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Few examples of « Nanotechnology » fields

– Nano-electronic: Electronic at nanoscale, it is a

prolongation of microelectronic field

– Nano-mechanic: Mechanic applied to nano-

systems or nano-objects

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 – Nano-electronic example : Nano-transistor
Characterisation of Fields Effect Transistor

UGs
Insulator

Gate

Moore Law: dimension evolution of transistor dimension

Uds Conductive
channel
Conductive transistor (switch on) : State 0
Blocked transistor (switch off) : State 1
Gate size

Etching
Other type of Nanotransistor

/ Year

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 - Nanomechanic: Mechanic applied to nano-systems or
nano-objects
Working Principle of an accelerometer in an F=Ma = KΔx F : force ; M : mass
𝛾: acceleration
embedded system (Mobile phone) ΔCi # ΔF K: spring constant
X x: position

K K
(M) (M)

MicroElectroMechanical System
MEMS & NEMS Interdigitalal combs Gyroscope MEMS

DOI:10.1109/MEMSYS.2006.1627738

Large areas with a low roughness at the nanoscale with plane

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surfaces face to face, are favourable aspects to surface effects
Surface/Volume ratio evolution
Total number Atoms at the
of atoms surface (%)

Surface effects compete

with volume effects

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 Evolution of surface-volume ratio

The sphere is the geometrical shape that

exhibits the smaller surface/volume ratio
1/C, surface/volume ratio (cm-1)

Bacteria Sphere Surface : 4π R2

Ameba Sphere Volume : 4/3 π R3 Rapport
Compacity : C=V/S= R/3
Hydra surface / volume 1/C= S/V= 3 / R
Fly To keep a high ratio of surface/volume, a
Earthworm
cut-out (inhomogeneous) shape is required.
salmon
Human

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 Forces acting at nanoscale in air environment

! ! ! ! !
Ft/s = FE/M + Fcap + FVdW + Frep
Sample sphere distance
Magnetic force
Fmi= Vi μ0 Mi (H)ÑH (z) Long-range
Electrostatic Capacitive
Force (1<n<2) interactions
1 ∂C 2 1 ε0εr S 2
Felect = U  n
U z ≈ 20nm
2 ∂z 2 z

Fcap = f (g , R,q p / eau , q eau / surf , z ) Capillary force

z≈ 5nm
HaR
FVdW ( z ) = Van der Waals Force
A 6z 2
Frepulsive ( z ) = z< 0.5nm
zm Repulsive force(m>3)
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Why the beach sand glues to the skin ?
Surface effect
SEM Image of sand grain

Let’s modelling the

sand grains as spheres

Effect of the capillary force

Modelling of Fcap Fcap versus the weight P
P
between two spheres

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Cours BUT GEII
 Impact of these forces on a sphere closed to a surface
The impact of the weight P : F : surface forces
! !
! = !" = !!" = ! !
!! !!
P : Weight force; V: sphere volume, R sphere radius;
ρ: volume density of the sphere material P
g : nominal gravitational acceleration

From the fundamental principle of mechanics : ! + !!!" = 0

Capillary force Fcap between a flat surface and a
sphere with a free-roughness surface

Water
meniscus

γ : liquid water surface tension

θ: contact angles 18
 Capillary force Fcap versus weight P
How a perfect gold (micro)sphere (roughness-free) can stick
on a perfect flat roof in air?
! + !!!" = 0
Substrate : perfect gold plane
Capillary vs weight
F(mN)
!! Θ = 0°
R γ : surface tension : 73mJ
! Θ: contact angle
Θ = 60°
Capillary force:

!!"# = !"#$%&'(

0 R(mm)
!
! = !" = !!" = ! !!! !!
!

In air the capillary force can be stronger than the weight for
sphere with a radius of several hundred of microns 19
 Van der Waals force versus weight
How a perfect gold (micro)sphere (roughness-free) can stick
on the gold plane roof in vacuum ?
Van der Waals force and Weight in function
Van der Waals force: substrate F(pN) of sphere radius
!!"#
HaR R
FVdW ( z ) =
6z 2 !
Ha : Hamaker constant of gold in vacuum # 4*10-19J
Z=100nm
12pN
! !
! = !" = !!" = ! !
!! !!

ρAu= 1.93*104 kg/m3 2.5μm

R(μm)
0
In vacuum, Van der Waals force can be stronger than the
weight for sphere with a radius up to few microns
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 Two main issues:

• How to observe (very) small objects individually ?

• How to measure forces acting at micro/nano-scale ?

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 Human eyes

microwaves

Hair diameter

Biological cell

Infra-red Red blood cell

Bacteria
Optical microscope
Visible lights
X-ray
microscope

Ultraviolet
protein
Electronic microscope Scanning probes
amino acid
X-Ray
atoms 22
Instrumental techniques to observe samples
from micron to nanoscale in direct space

1. Optical and fluorescene microscopy (fluo: E. Planus)

2. Scanning tunnelling microscopy (Local probe course)
3. Atomic force microscopy
4. SEM and TEM (Fabien Dubois course)

The main aim of the microscopy is to observe objects too small to

be visible with human eyes by producing enlarged images of them.

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 Radiations
Infrared
X ray Radio waves

wavelength

Spectrum of electromagnetic radiation

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Description of a modern optical microscope

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A key element : the microscope objective.
How to understand its parameters ?

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Example of optical image an SEM Image

Optical image Image obtained by SEM

The classical optical microscope is limited in resolution i.e. the

possibility to distinguish two objects separated by a distance ‘d’.

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 Resolution of classical optical microscopy: Rayleigh criteria
Resolution: minimal gap between two objects required to distinguish
them with a classical optical microscope.
For small and circular objects, A and B in the illustration
(i.e. theory of light diffraction by slits), their respective images A’ and B’ due to the light
diffraction could be distinguished (and by the way measured) if :

With d lens diameter, 𝝺 the light wavelength

S θ
as AB = A'B’.l / l’,
Light source (S) the previous conditions become:

Lens

As in most cases, the ratio (l/d)> 1, the

resolution reaches at its best the wavelength
of the used light.

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 Illustration of the Rayleigh criteria
For two points A and B, the evolution of their image A’ and B’ according to their distance

collection
Collection of Views in:
of points
spots in 2D view 2D
S
and

3D
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 Resolution of a real classical optical microscope
Towards camera or eyes piece Figure 2

D = λ/2n(sin(α))
Figure 1
D = λ/2NA
n is the optical index of the working environment; α: angle of the light cone
λ : light wavelength; D: distance between two points on the sample
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NA: Numerical aperture;
Impact of the NA on image quality and
resolution
d = λ/2n(sin(α))
d = λ/2NA S

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 ‘Ultimate’ lateral Resolution of an optical
microscope
Exercise: Calculate the theoretical ‘ultimate’ resolution of an
optical microscope working in air using red and violet light and
having a NA equals to 1

dlimit = λ/(2nsin(α))= λ/2NA

dlimit (Violet) = 400/2= 200nm
dlimit (red) = 800/2= 400nm

How to improve this resolution ?

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 Immersion classical optical microscope

If the sample and the objective lens are immersed in oil, therefore the working
environment index increases and the wavelength can be expressed as ln = l/n

λn 500 ×10−9
d min = = = 1.67 ×10−7 m = 0.167um
2 NA 2 ×1.5×1 Resolution improved by a Factor of 2
compared to air
To go further: http://www.microscopyu.com/
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Vertical resolution of a classical optical microscope:
Depth Of Field (DOF)

DOF

The DOF decreases when the NA increases.

Ex: DOF = 2.5μm with ×10 objective (NA=0.3)
while
DOF = 0.55μm with ×100 immersive objective (NA=1.4)
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 Working Distance (WD)

DOF =

WD
DOF : ΔZ

For the best objectives(1<NA<1.4)

WD about few hundred of 𝝁m up to few mm
For the high magnification, the rugosity of the
sample surface must be low compared to the WD!
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 Toward the Nanoscopic scale…

Classical optical microscopy Others types of microscopy

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