Introduction in Atomic Force Microscopy

How can we see very small things?

shape
size

information
T

- light
- electrons

surface

image
color

11:25

(geometrical representation)

Introduction in AFM

What is scanning probe microscopy?

How SPM help us to see very small things

Scanning probe microscopy techniques resemble the way

of how blind people get images about things. They explore
the thing surfaces by touch.
In scanning probe microscopy a sensitive tip explores the
surface of a micro or nano object in the same way as a
stylus profilometer get the profile of a sample surface.
tip
image
surface
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Introduction in AFM

How a tip probes the surface of a sample ?

FIELD EMISSION EFFECT (1972

TUNNELING ELECTRON CURRENT INTENSITY

G. Binnig, H. Rohrer, C. Gerber, E. Weibel
Surface Studies by Scanning Tunneling Microscopy
Phys. Rev. Lett. 49 (1982) 57.

STM

surface

tip

R.D. Young, J. Ward, F. Scire,

Rev. Sci. Instrum. 43 (1972) 999.

I exp( c d )

sample
O

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Introduction in AFM

How a tip probes the surface of a sample ?

tip

ATOMIC AND MOLECULAR FORCES

G. Binnig, C.F. Quate, C. Gerber
Atomic Force Microscope
Phys. Rev. Lett. 56 (1986) 930.

surface

1
F n
d

AFM

sample

d
FVdV

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Introduction in AFM

AR
d2
4

How a tip probes the surface of a sample ?

tip

INTENSITY OF REFLECTED LIGHT (1984)

SCANNING NEAR FIELD OPTICAL MICROSCOPY
D. W. PohlW. Denk, M. Lanz, Appl. Phys. Lett. 44 (1984) 651

surface

SNOM
I

1
d4

sample
O

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Introduction in AFM

Principle of the STM operation

The tip is approached to sample
surface until the tunneling current

(x, y, z)
piezoelectric
actuator

x
y

(x, y) scan
control
unit

reaches certain preset value.

0.2 to 10 nA

Then, the tunneling current is is

kept constant during the scan by a
feedback unit that controls the tip
height, z, through a piezoelectric
actuator. The sample surface is
raster scanned in a (x, y) plan
parallel to the sample surface.

11:25

It

sample

feedback
control
unit
+
U

10 mV to 1V

sample
stage

Introduction in AFM

Principle of the STM operation

It = const.

Depending on the feedback gain,

the STM may operate in one of
the either constant-current mode
or constant-height mode.

z(x, y)

tip
z = variable

x
y

sample

High feedback gain

It = const. mode
It = variable

Low feedback gain

z = const. mode

It (x, y)

tip
z = const.
d
x
y

sample

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Introduction in AFM

Principle of the AFM operation

G. Binnig, C.F. Quate, C. Gerber,
Atomic Force Microscope,
Phys. Rev. Lett. 56 (1986) 930.

STM
Z PZT

FORCE SENSOR

STM
feedback
control unit

It

+
STM
tip

kN

FN
E b h

z (l )
4 l

kN = 50 N/m

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AFM
tip

sample

m odulating
piezo

X,Y,Z scan

Introduction in AFM

Detection of cantilever deflection system

(optical lever)
force sensor
laser

w/2
leff
l

+
-

OA

normal force
signal
cantilever base

photodiode

E b
h
kN

2 l 2 w 2 / 4 1/ 2

kN = 0.1 - 1 N/m

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cantilever

Introduction in AFM

Detection of cantilever deflection system

(piezoelectric sensor and tuning fork)

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Introduction in AFM

10

Manufacturing the AFM probes

Low effective mass
high resonant frequency (> 10KHz)
small elasticity constant (0.1-1 N/m)
high quality factor ( 104 in UHV)
good light reflectivity
sharp tips (10-50 nm)
Silicon microfabrication
S. Akamine, R. C. Barrett, M. J. Zdeblick, and C. F. Quate,
A Planar Process for Microfabrication of a Scanning
Tunneling Microscope,
Sensors and Actuators A21-23 (1990) 964.

Pyrex
glass

3.5
mm

0.5
mm
Si 3N4
0.1-0.2 mm

Au
35
o

(111)
35
o

(110)

(100)
3-4 m

S. Akamine, R. C. Barett, and C. F. Quate,

Improved AFM images using microcantilevers with sharp tips,
Appl. Phys. Lett. 57 (1990) 316.

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Introduction in AFM

11

Commercial AFM probes

triangular

single-beam

silicon triangular pyramidal tip

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Introduction in AFM

12

AFM tip characteristics

TEM image of a carbon nanotube

attached to the AFM tip

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Introduction in AFM

13

Scan system: the piezolelectric tube

t

lead zirconate titanate cylindrical

tube with one inner electrode and
four outer electrodes
PIEZO

l2
x, y, z Vx , y , z d 31
t d
x

-x

+x

elongated

contracted

-y

+Vy

+y
+x

-Vx

-x
d

-y

fixed base

+Vx

-Vy

+Vx
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Introduction in AFM

14

-Vx

Block diagram of the AFM

force detector
(F)
z
sample

-x
-y
+
y

feedback loop

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-digital
-analog

Introduction in AFM

preset force
value
(F0)

PC
DAC

x scan

+
x

error
signal

y scan

subtraction
stage
(F-F0)

ADC

z signal

PIEZO

The force signal from the force detector is

fed into the feedback loop consisting of
subtraction stage that yields the error
signal, which is the difference between the
preset force and the detected force. The
error signal is integrated to remove high
frequency noise and is fed to a correction
block to set the voltage that has to be
applied to the z actuator in order to keep
constant the tip-sample interaction force.

z+
y
-y high voltage
amplifier
-x
+
x

15

How an AFM image is acquired

(a)

(b)
fast scan direction

j
y

j+1

x, y

backward

forward

i+1

forward

backward

X
Y

N 1 N 1
z(x)
10

-10
0

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200

400
600
x [ nm ]

800

1000

Introduction in AFM

16

slow scan direction

xY

slow scan direction

zi, j

fast scan direction

Contact mode of AFM operation

approach
retract

15
10

working point

5
a

0
-5
-10
-15

-20

tip

sample
(c)

20
tip-sample interaction force [ nN ]

-40

-60

-80

-100

sample height [ nm ]
(z)

k = 0.57 N/m

N
approach
retract

15
10

jump into contact

5
0

attractive

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jump out of contact

-20
20

sample

jump into contact

f

attractive

(b)

repulsive

sample

tip-sample interaction force [ nN ]

20

repulsive

(a)

-5
-10
jump out of contact

-15
-20

Introduction in AFM
0

17
20

40

60

tip-sample distance [ nm ]

80

100

Role of the cantilever stiffness. Capillary

condensation

soft

0
-5
-10
-15

jump out of contact

-20

tip

120

repulsive

20

tip-sample interaction force [ nN ]

jump into contact

f

-20

-40

-60

-80

-100

sample height [ nm ]
(z)

kN = 0.57 N/m
c

approach
retract

100
80
60
40
jump into contact

20
a

0
-20
-40
20

11:25

working point

140

sample

approach
retract

10

sample

stiff

15

attractive

tip-sample interaction force [ nN ]

20

f
d b

Introduction in AFM

-20

-40

-60

sample height [ nm ]

k = 15 N/m

-80

18

Lateral force microscopy (LFM)

-0.07

advance
recede

advance

recede

lateral signal [ V ]

-0.08
Ffr (advance)
-0.09
null lateral force line
-0.10

Fz
Ffr (recede)

Fx

Fz
Fx

-0.11

500

1000

1500

2000

advancin or receeding distance [ nm ]

F fr

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A fr
2d

Introduction in AFM

19

How is measured the lateral force?

lateral
deflection

laser
beam

vertical
deflection
+

vertical
signal

lateral
deflection

vertical
deflection

+
-

lateral
signal

vertical
deflection
torsion

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Introduction in AFM

20

Dependence of the friction force on the

sample chemical composition
tip couvered by
functional
m olecules
terminated with
COOH group

tip couvered by
functional
m olecules
terminated with
CH3 group

tip

tip

C. D. Frisbie, L. F. Rozsnyai, A. Noy,

M. Wrighton, C. M. Lieber

Science 265 (1994) 2071.

Chemical Force Microscopy

-COOH

-CH3

-CH3

-CH3

-COOH

-COOH

high friction

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-COOH

Introduction in AFM

-CH3

low friction

21

Dependence of the friction force on the

sample chemical composition?
Au

Au
Si(100)

lateral signal [ mV ]

Si(100)

z [ nm ]

40

Topography image

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RH 40

30
20
600
400
200
0
0

200

400

600

800

1000

Friction force image

Introduction in AFM

22

1200

Dynamic force Microscopy

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Introduction in AFM

F(d)

sample

sample

Working in contact mode may deform or even

destroy soft surfaces as those of polymers or
F(d)
biological samples.
To investigate the topography of soft samples
a non-contact AFM mode, which employs the
long-range tip-sample interaction forces to
determine the sample height, should be used.
The non-contact AFM modes use a vibrating
AFM tip to explore the sample surface. When
such a vibrating tip approaches a sample
surface, the amplitude, frequency and the
phase of the oscillations change and this
changes are used by a feedback loop to
determine the sample surface height.
excitation
This technique is called dynamic force
microscopy (DFM).
Non-contact mode

excitation

Tapping
intermittent contact mode
23

Operation modes. Analogy with the

harmonic oscillator
0

kz
meff

100

amplitude [ a. u. ]

eff 0 1 Fz / z / k z
surface

AFM

1
dn
d
FVdV

repulsive
11:25
Intermittent
contact

80
60
40
20

Vz
0
z

no external force
attractive
repulsive

0
0.8

AR
d2

1.0

1.1

1.2

/ 0

vacuum: Q = 104
air: Q = 50-200
liquid: Q = 2-50

Vz
F
0, z 0
z
z
atractive
Non-contact

0.9

Introduction in AFM

24

Operation modes. intermittent contact

and non-contact modes

intermittent

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non-contact

Introduction in AFM

25

Cantilever quality factor

vacuum: Q = 104
air: Q = 50-200
liquid: Q = 2-50
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Introduction in AFM

26

Working in liquid environment. Thermal

noise frequency power spectrum

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Introduction in AFM

27

Amplitude curve

Typical amplitude curve

in air.
The sample surface is
detected by the decrease of
the tip oscillation
amplitude

oscillation amplitude [ nm ]

15.0

approach
retract

14.5

14.0

13.5
intermittent-contact
13.0
0

-20

-40

-60

-80

-100

sample height [ nm ]
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Introduction in AFM

28

Dependence of the phase lag on energy

loss: case of the harmonic oscillator
180

Qeff

W0
2
Wl

140
120
100
80
60

100

40
20
0

11:25

90

0
/ 2 2 Qeff
0

Q = 100
Q = 500

160

phase lag [ deg. ]

( 0 ) / Q
tan( )
02 2

500

180
0.96

Introduction in AFM

0.98

1.00
/ 0

1.02

1.04

29

Dependence of the phase lag on

surface chemical composition
Topography image

Phase lag image

Au
Si

Au
Si

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Introduction in AFM

30

Dependence of the phase lag on

surface structure and topography
Topography effect
Variations of the
phase lag occur
mainly at the grain
borders

Effect of the
crystal structure
The contrast in the
phase lag is due to
composite crystal
structure of the
surface

(dark -rutile TiO2)

(light -amorphous TiO2)

11:25

Introduction in AFM

31

Choosing the right cantilever

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Introduction in AFM

32

Force curve mapping

All important information on sample
surface properties and forces is contained
by the tip-sample force curves.
If force curve data are digitally acquired
for a number of points homogeneously
distributed on a sample surface, then these
data can be digitally processed to extract
the relevant information on the sample
surface properties. This technique is called
force curve mapping (FCM)
FCM provide simultaneously imaging of
sample topography along with other
important sample properties, as surface
stiffness (elasticity), viscosity, adhesion
force, shear force, chemical composition ,
etc., at the atomic or nano scale.
11:25

approach
retract

PC
z
x

Z piezo
driv er

y
LASER

PHD

sam ple
X, Y piezo drivers

Memory = 128 x 128 x (2 x 128) x 2 bytes

Introduction in AFM

33

Acoustic mode AFM

11:25

Introduction in AFM

34

AFM as a biologic sensor: shift in

resonant frequency

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Introduction in AFM

35

Plane correction. Image flattening

Surface tilted in both x and y directions

x
y
Surface after correction along y
direction, still tilted in x direction

y
x
Surface after correction along x and y
directions
x
y
11:25

Introduction in AFM

36

Widening small objects: lateral versus normal resolution

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Introduction in AFM

37

Lateral resolution

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Introduction in AFM

38

Effect of tip shape: double tip

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Introduction in AFM

39

Effect of feedback on the topography image

correct feedback

slow feedback

too fast feedback

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Introduction in AFM

40

Further reading

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Introduction in AFM

41