Characterization 2005-05-02

Characterization of Thin
Primary Secondary
Energy range Acronym Technique Application
beam signal

Electron
20 - 200 eV LEED Low-
Low-energy electron diffraction Surface structure

Films
Electron
0.3 - 30 keV SEM Scanning electron microscopy Surface morphology
X-ray
l - 30keV EMP Electron microprobe Surface region composition
Electron
Electron 500eV-
500eV-10keV (EDX) AES Auger electron spectroscopy Surface layer composition
Electron
100 -400 keV TEM Transmission electron microscopy High-
High-resolution structure
Electron, X-
X-
100 -400 keV STEM Scanning TEM Imaging, X-
X-ray analysis
ray
100 -400 keV EELS Electron energy loss spectroscopy Local small-
small-area composition
Electron
• Film thickness
• Surface morphology 0.5 -2.0 keV Ion ISS Ion-
Ion-scattering spectroscopy Surface composition
• Film composition 1 - 15 keV Ion SIMS Secondary ion mass spectroscopy Trace composition vs depth
1-15 eV Atom SNMS Secondary neutral mass spectrometry Trace composition vs depth
• Film properties Ion
1 keV and up X-ray PIXE Particle-
Particle-induced X-
X-ray emission Trace composition
5-20 keV Electron SIM Scanning ion microscopy Surface characterization
Characterization methods are very diverse >1 MeV Ion RBS Rutherford backscattering Composition vs depth

>1 keV X-ray XRF X-ray fluorescence Composition (1 m depth)

depth)
• Size of equipment. Compare desktop interferometer with 2 m accelerator of RBS >1 keV X-ray XRD X-ray diffraction Crystal structure
Photon >1 keV Electron ESCA, XPS X-ray photoelectron spectroscopy Surface composition
• Cost. $101 – $106 Laser Ion - Laser microprobe Composition of irradiated area
• Environment. Ambient – 10-10 Torr Laser Light LEM Laser emission microprobe Trace element analysis
• Complexity. Scotch tape – SEM, TEM etc.

J.B. Bindel, in VLSI Technol, McGraw-Hill, NY88

1 2

FILM THICKNESS

1000000 Optical methods Mechanical methods

TEM

Interferometry Ellipsometry
EMP(EDX)

100000
AES

STEM

SIM
EELS

SIMS

• reflection • reflection
PIXE

• Profilometry
SEM

10000
Energy (eV)

ISS

• spectral • spectral • Quartz crystal microbalace

1000
LEED

• Ultrasound
100
• elegant
SNMS

• non-destructive
10
• high-resolution
• fast
1 • easy to implement
electrons ions

3 4

FILM THICKNESS FILM THICKNESS

Optical methods Multiple-beam reflection
Method Range (nm) Characteristics (M = multiple)
Multiple beam
3 - 2000 ± 1-3 A step and reflective coating required (1 , = 90°
90°)
interferometry (FET)
FET)
Multiple beam A step, reflective coating, and spectrometer
1 - 2000 ± 0.5
interferometry (FECO)
FECO) required; time consuming (M )
VAMFO (variable-
variable-angle 80 - 1000 ± 0.02-
0.02-
monochromatic fringe Transparent films on reflective substrate (1 , M )
0.05%
observation)
CARIS (constant-
constant-angle Transparent films on reflective substrate (M , =
reflection interference 40 - 2000 ± l nm
spectroscopy)
90°
90°)
spectroscopy)
Transparent films and multilayers, uses polarized
Ellipsometry <0.1-
<0.1-
light, measures d, n, and k (1 , fixed )
Transparent films and multilayers, fast, measures
Spectral reflectometry ~ 30 - 2000±
2000± 1 d, n, and k ( = ~ 200-
200-1000 nm, = 90° 90°)
(unpolarized)
unpolarized) nm (polarized reflectometry is also performed at l , M
)
Transparent films and multilayers, uses polarized
Spectroscopic
<0.1-
<0.1- light (M , fixed ) (multiple-
(multiple-angle ellipsometry is
ellipsometry
also performed at l ) Fringes of equal thickness
Fringes of equal inclination
5 6

August Yurgens 1
Characterization 2005-05-02

Interferometry: fringes basics Interferometry: fringes basics

E. Hecht, Optics (Addison-Wesley, 98)

optical path difference = n f (AB + BC) − n1 AD

d
2d
AB = BC = d / cos θ t → = nf − n1 AD
cos θ t
nf
AD = AC sin θ i ; AD = AC sin θ t ; AC = 2d tan t
n1 X
2d due to reflections Fizeau, Armand (1819-1896)
= nf (1 − sin 2 θ t ) = 2dn f cos θ t
cos θ t
(speed of light)
4π n f
relative phase shift δ = k0 Λ ± π = cos θ t ± π =
λ0 d = xα , and for small θ i :
4π d E. Hecht, Optics (Addison-Wesley, 98) (m + 1 / 2)λ0 = 2n f d m or
= n 2f − n 2 sin 2 θ i ± π
λ0 (m + 1 / 2)λ0 = 2α xm n f
δ = 2 mπ → Fringes of equal thickness
δ = 2 mπ → λ0
λ0 xm +1 − xm = = fringe spacing (Fizeau fringes)
λ0 d cos θ t = ( 2m + 1) (maxima) 2α n f
d cos θ t = ( 2m + 1) (maxima) 4n f
4n f Fringes of equal inclination
λ0 d cos θ t = ( 2m)
λ0
(minima)
nf 1 for air FET
d cos θ t = ( 2m) (minima) 4n f
4n f
7 8

FILM THICKNESS- Optics FILM THICKNESS- Optics

Multiple-beam reflectometry: Multiple-beam reflectometry:
non-transparent films non-transparent films

∆ λ
d=
Fringe spacings 2
For highly reflective surfaces, the fringe width is ~1/40 of , and ~1/5 of that can be
detected the resolution is about 1/400 of , i.e. ~15 Å
9 10

FILM THICKNESS- Optics FILM THICKNESS- Optics

Transparent films Multiple-beam reflectometry
...with a scanner

fringes

glass disk
in the scanner

fringes

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August Yurgens 2
Characterization 2005-05-02

FILM THICKNESS- Optics Spectral Reflectometry FILM THICKNESS- Optics

Transparent films and multilayers, fast,
measures d, n, and k ( = ~ 200-1000 nm, Spectral Reflectometry
= 90°)
http://www.filmetrics.com/pdf/TMO.pdf
http://www.filmetrics.com/
Patterned-Wafer Thickness and Defect
Mapper
The STMapper uses a new scanning technique
to acquire millions of spectral reflectance data
points on a 200mm wafer in less than five
seconds. An entire cassette of wafers can be
mapped in less than five minutes. It can be used
to monitor multiple process parameters on
patterned wafers, such as ILD thickness, metal
residual, and scratches and defects. Available in
integrated or stand-alone configurations.

13 14

Ellipsometer - Rudolph AutoEL-II

Ellipsometer - Sagax Iscoscope #105
Ellipsometry:
FILM THICKNESS- Optics • reflection ellipsometry
• multiple angle of incidence
• spectroscopic ellipsometry
#104
Light source Light source
te

te
pla

pla
Detector Detector
r

r
ve

ve
ize

ize
wa

wa
lar

lar
Po

Po
er

er
art

art
Qu

Qu

NULL NULL

in situ measurements Analyzer in situ measurements Analyzer

complex reflection coeff. complex reflection coeff.

ρ = tanψ exp(i∆ ) ρ = tanψ exp(i∆ )

A typical experimental setup in ellipsometry A typical experimental setup in ellipsometry

15 16

FILM THICKNESS Spectroscopic ellipsometry FILM THICKNESS- Mechanics Profilometry

(one-shot AFM)
complex reflection coeff.
deflection measurements
ρ = tanψ exp(i∆)
(interferometry, capacitance, etc...)
resolution: ~1Å
deflection (Å)

spring
0.1-50 mg

lateral distance ( m) • tip angle 45 or 60°

• tip radii 0.2-25 m

thin film

• scratching of thin film

substrate • substrate roughness
in situ measurements during thin film growth • vibrations
17 18

August Yurgens 3
Characterization 2005-05-02

Quartz Crystal Quartz Crystal

FILM THICKNESS- Mechanics Microbalances FILM THICKNESS- Mechanics Microbalances

SiO2
Rock crystal

clock crystals
AT

= K/M
K
f 2 δm f 2d • f = 6 MHz typical (AT cut, thickn. shear)
δf =− =−
• temperature sensitive (-)
C ρf A C

M C=1656 kHz mm (AT cut)

Ametist 13.9 x 10.6 x 8.3 cm3, ~1 kg 19 20

FILM THICKNESS- Acoustics Ultrasonic methods FILM THICKNESS- Acoustics Ultrasonic methods

time delay

second pulse first pulse

probes the change excites (heats)
in surface reflection the surface

local heating local sudden expansion

acoustic wave pulse interface
change of reflection at the surface

ultrasound reflected from the interface21 22

SEM
STRUCTURAL CHARACTERIZATION STRUCTURAL CHARACTERIZATION

MC2’s SEM SEM

JEOL JSM-6301F SEM

Installed: 1994
Funded by: Wallenberg
Max sample size: 100 mm
resolution 1.2 nm specified
Acc. voltages 0.5kV - 30kV
Source: Cold Field Emission

23 24

August Yurgens 4
Characterization 2005-05-02

Large SEM Jeol SEM

STRUCTURAL CHARACTERIZATION STRUCTURAL CHARACTERIZATION

http://www.jeol.com/sem/gallery
25 26

STRUCTURAL CHARACTERIZATION STRUCTURAL CHARACTERIZATION

125 – 300 keV (up to 1 MeV) short wavelength
TEM 100 keV 0.035 Å TEM
http://www.fzu.cz/~vystav/TEMpage.html TEM cross sections
HRTEM: of coherent twin in molybdenum
Microscope: JEOL 4000EX
(CEA/DRFMC Grenoble)
http://www.fzu.cz/~vystav/TEMpage.html

magnetic domains in Co

TEM modes: TEM modes:

• Bright-field imaging • Bright-field imaging
• Dark-field imaging • Dark-field imaging
• Lattice imaging • Lattice imaging
• Diffraction • Diffraction
• X-ray spectroscopy • X-ray spectroscopy
• Electron energy loss spectroscopy • Electron energy loss spectroscopy
• Lorentz microscopy 27
• Lorentz microscopy 28

STRUCTURAL CHARACTERIZATION STRUCTURAL CHARACTERIZATION

FIB
microscopy X-ray
• Voltage contrast: insulators look dark
diffraction
while conductors are bright
• Materials contrast: differences in yield
Monitoring of interdiffusion in thin films Epitaxial thin films
of secondary particles
• Crystallographic orientation contrast
(channeling contrast)

A grain-size distribution can be deduced

29 ! 30

August Yurgens 5
Characterization 2005-05-02

STRUCTURAL CHARACTERIZATION CHEMICAL CHARACTERIZATION

STM • SEM/EDX (energy dispersive X-ray

capable of detecting almost all
• AES (Auger electron spectroscopy)
elements of the periodic table
• XPS (X-ray photoelectron spectroscopy)
http://www.fysik.dtu.dk/stm/instrument.htm • RBS (Rutherford backscattering)
• SIMS (Secondary-ion mass spectroscopy)

STM allows manipulation

of individual atoms

Fe on Cu
31 32
Crommie, Lutz & Eigler in http://www.almaden.ibm.com/

CHEMICAL CHARACTERIZATION CHEMICAL CHARACTERIZATION AES energies

these can be collected and analyzed
(XPS or AES)

33 34

CHEMICAL CHARACTERIZATION AES CHEMICAL CHARACTERIZATION

these can be collected and analyzed

35 36

August Yurgens 6
Characterization 2005-05-02

Films
CHEMICAL CHARACTERIZATION CHEMICAL CHARACTERIZATION

Auger Electron Spectroscopy (AES) X-RAY PHOTOELECTRON SPECTROSCOPY (XPS)

• The sample is irradiated with a high energy primary electron beam (2 - 10 keV).
• Backscattered, secondary, and Auger electrons can be detected and analyzed.
These can also be used for imaging purposes similar to that in SEM.
• The Auger electrons are emitted at discrete energies, that are characteristic of the
elements present on the sample surface (the peak positions are used to identify the
elements and their chemical states) All elements in the periodic table, except
hydrogen and helium, can be detected, and
• The depth of analysis is 3 - 5 nm
• In the scanning mode, the secondary electrons yield information on the surface
topography. Excellent spatial resolution (0.5 m).
also Electron Spectroscopy for Chemical Analysis (ESCA)
• The sample is irradiated with soft X-rays photons (1-2 keV) which induces direct
emission of photoelectrons.
• The energy of photoelectrons is characteristic of the material.
• Depth 2-20 atomic layers.
• Peak position and area are used to study the composition. The peak shape give
information about the chemical bonds of the elements.
Modes of Operation
1. Energy spectrum. Survey spectra (0-1000 eV) - to estimate the composition,
while high-resolution spectra (10-20 eV) - information about the chemical bonds.
2. Mapping. Choosing a single peak and scanning the focal point across the
sample gives information on the lateral distribution of species on the surface.
3. Imaging with high spatial resolution (<10-15 m) and high sensitivity.

• Top layers can be spattered with ions and depth profiles can be measured.
37 38

CHEMICAL CHARACTERIZATION CHEMICAL CHARACTERIZATION

Secondary Ion Mass SpectroscopyDescription (SIMS)

The most sensitive method for detection of elements.
• masses up to 104 mass units can be detected;
XPS vs AES (are complimentary to each othe)
• separation of isotopes can be made;
• Give similar information.
• chemical information can be obtained by identifying sputtered ions;
• detection limits of 1 ppm of a monolayer;
• The Auger spot size is smaller than the XPS.
• surface sensitivity < 1nm; depth resolution < 1nm; lateral resolution 100 nm.
• The XPS spectra are well-documented -> study of surface
Modes of operation:
chemical bonding through the use of tabulated chemical shifts. The
1. Surface analysis – (Static SIMS) - low primary ion densities to prevent
Auger chemical shifts are weaker.
surface destruction
2. Imaging. Focused ion beam scanning over the surface produces images of
• X-rays produce less damage to the surface compared to the
the surface (recall FIB !)
primary electrons of AES.
3. Depth profiling (Dynamic SIMS) - high primary ion dose densities to remove
the surface layer by layer. Spectra taken during the sputtering can give the
thickness distribution of elements

39 40

CHEMICAL CHARACTERIZATION CHEMICAL CHARACTERIZATION

SIMS

http://hyperphysics.phy-astr.gsu.edu/hbase/magnetic/maspec.html

The mass spectrometer is

an instrument which can
measure the masses and
relative concentrations of
atoms and molecules.

It makes use of the

magnetic force on a
moving charged particle.

41 42

August Yurgens 7
Characterization 2005-05-02

CHEMICAL CHARACTERIZATION RBS CHEMICAL CHARACTERIZATION RBS

Easiest to understand: two-body elastic scattering

Rutherford backscattering is an analytical technique in which a high energy

beam ( 2 - 4 MeV ) of low mass ions (He ++ ) is directed at a surface. A
detector collects particles which scatter from the sample at close to a 180
degree angle.

•The energy of scattered ions depend on their incident energy and on the mass
of the sample atom which they hit. The energy of scattered ions therefore
indicates the chemical composition of the sample.

•RBS can be used to perform a depth profile of the composition of a sample.

This is especially useful in analysis of thin-film materials.
2
M 2 − M 02 sin 2 θ + M 0 cos θ
E1 = E0
M0 + M
E1 = K M E0

43 44

Properties of Thin Films Properties of Thin Films

Mechanical Properties Deflection of microbeams

45 46

Properties of Thin Films Properties of Thin Films

Indentation Bulge testing

Nano indentation test can be used in the analysis of organic and inorganic soft and 4dh 2 E h2
P= σ0 +
hard coatings. Examples are thin and multilayer PVD, CVD, PECVD, photoresist, and r2 3 1 −ν r 2
many other types of films. Substrates can be hard or soft, including metals,
semiconductors, glass, and organic materials. σ 0 - residual stress
h - dome height
47 48
r , d - radius and thickness

August Yurgens 8
Characterization 2005-05-02

Properties of Thin Films Properties of Thin Films

Measurements of Internal Stresses Adhesion Tests

49 50
!"!#

Properties of Thin Films Properties of Thin Films

Electrical resistivity
Improving ADHESION electrical current : J = nev
v = µ E ( µ - mobility)
* + '+

$ ,-
E
J = neµ E = σ E = $. ' /0
$% ρ 0
(Ohm' s law) $1
$& ' $2 '
$( $2 0
$& '
$)

51 52

Properties of Thin Films 3

Properties of Thin Films

Electrical resistivity
measurements ((45#

'+ 6 78

/
53 ' 54

August Yurgens 9
Characterization 2005-05-02

Properties of Thin Films Properties of Thin Films

((45#

* '
+ 0
' +
/ ,-
'

/
55 56

Properties of Thin Films - Properties of Thin Films -

F= 5 Å for Cu, but

F = 400 Å for Bi (!) λF = 2π / k F -
- π
pz = n, n = 1,2,3...
a
ε ( p|| , p z ) = ε

/
9

-
+-
p||2 π2 2
ε= + n2
2m|| 2m z a 2
+ π2 2
∆ε n, n+1 = (2n + 1)
+9 2mz a 2
1
#.:' 9 < +
0; 0(' 57 58
a quantum box

Properties of Thin Films = ( Properties of Thin Films

((45# . 8>88'
?
2

/
59 60

August Yurgens 10
Characterization 2005-05-02

Properties of Thin Films Properties of Thin Films

<+
<

<
@

' /

61 62

Properties of Thin Films Properties of Thin Films

D 8!! / E2- < F;.

A8! B C4 D 8!! / E2- < F;.

, &
, )4!!# + & 8

-G 4 4

2 / 63
+ G =HG
64

August Yurgens 11