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Metallic multilayers
Metallic multilayers are composed of two very thin different materials
layers alternatively. These layers can vary from a few to more than
thousands individual layers, thickness range from a few atom to a
thousand atoms and the corresponding maximum structure thickness
could be of about 10 millionth of an inch
History
The first application of multilayers performed more than 60 years ago. In
the semiconductor industry for making hard disks and computer chips,
macro multilayers became an essential part. Then advances in fabrication
techniques took place and with the applications in the x-ray and
ultraviolet regions of the electromagnetic spectrum, we got more
advanced multilayers for the industry and for the research work. A new
class of telescope could be possible because of high reflectivity multilayer
mirrors, which is very useful for solar physics and astronomical
research .Multilayers optics have applications in electron microprobes,
scanning electron microscopes (SEM) and X-ray layers etc[7]
Properties of multilayers
Higher strength
Corrosion resistance
Heat resistance
Fracture resistance
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Better optical properties
1 Destructive Technique
Spectroscopic ellipsometry
Interferometry
X ray reflectometry
SEM,TEM,HRTEM all are imaging techniques ,so we can actually see many
layers of different metals and measure the thickness ,but sample
preparation is a difficult and time consuming task.[1]
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Formation of nanostructured metallic multilayers
Formation of nanostructures is based on mechanical deformation under
high strain rate and shear condition. Mechanical alloying of powder
particles has been used in preparing nanoscaled material with large range
of chemical composition and atomic structure. When a mechanical
deformation takes place there is a change in thermodynamic, mechanical
and chemical properties of these materials, which has been observed with
properties of nano phase materials. There are two methods of
nanostructure formation. [2]
The other method is high energy milling, which is a non equilibrium solid
state process which results in material with nano microstructures. [2]
In this report we will first discuss the non destructive techniques and how
to determine the thickness from that technique and then we will discuss
the destructive techniques and will compare the results and advantages.
λ = 2d sin θ
Basic principle
of XRD
In the figure
below the
diffraction angle
2θ is the angle
between incident
and diffracted x
rays. The
diffracted
intensity is
measured as a
function of 2θ and the orientation of the specimen. The x-ray wavelength
λ is 0.7 – 2 A˚ [1]
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Electron probe microscopy (EPMA)
Electron probe X-ray microanalysis (EPMA) is an elemental analysis
technique in which a specimen is bombarded with a focused beam of
energetic electrons. Beam energy is 5 – 30 keV. The X- rays are measured
by EDS or WDS X- ray spectrometers. EDS is energy dispersive and WDS is
wave length dispersive spectrometer. In this technique we can use
beryllium to actinides range of elements. This is a non destructive
technique and in rare cases there is a chemical bonding as well in EPMA.
Depth profiling is rarely by changing incident beam energy. Accuracy is
±40% relative in 95% cases in polished, flat sample. The detection limit in
WDS is 100 ppm and in EDS it is 1000 ppm. Sampling depth is dependent
on energy and matrix and it ranges between 100 nm- 5 µm. Lateral
resolution is also depend on energy and matrix, which ranges between
100 nm- 5 µm. EPMA is suitable for compositional mapping and SEM
imaging. [1]
The sample used in EPMA should be solid conductors and insulator, <2.5
cm in diameter and <1 cm thick, rough surface, thin film and polished flat
particles. The major uses of EPMA are in non destructive quantitative
analysis of major, minor and trace constituents of materials. The size of
EPMA instrument is 3m*1.5m*2m high. [1]
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Reflectance spectroscopy
In the reflectance spectroscopy the reflectance spectrum of a coated
sample is used to determine the thickness of a polymeric coating. Based
on the interference fringes observed, the thickness of the film is
calculated.
Where
d= film thickness
m= number of fringe
n= refractive index
θ= angle of incident
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Fig 2- Reflectance spectrum showing interference pattern from [4]
Interferometry
In the interferometry we use an optical interference system, which after
deposition allows us to determine the thickness of metallic films. In this
process we
compare the two
patterns
generated by the
substrate with and
without deposited
film on it. The
thickness of film is
determined by the
difference of
measure of
pattern. [6]
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Fig 3- Michelson interferometer used to measure the thickness from [6]
g = (a/b) (λ/2)
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Traditionally for the small scale material characterization first instrument
comes in mind is optical microscope but it gives limited results, for the
detailed result optical microscopes are replaced by scanning electron
microscopes and transmission electron microscopes .SEM gives the highly
magnified image of the surface of the material.SEM not only just provides
the information about surface region but it provides the information
concerning composition near the surface region of the material as well. [1]
High voltage TEM has better electron penetration because high energy
electrons interact less strongly with matter, so we can work with thicker
samples n a high voltage TEM.
1 diffraction mode
2 image mode
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Single crystal produces spot pattern and polycrystalline produces a ring
pattern. [1] and [3]
The image mode produces an image of the illuminated sample area. There
are several mechanisms to contain contrast to image i.e. mass contrast,
thickness contrast, and diffraction contrast and phase contrast.
The most difficult task in TEM is the specimen preparation, which is a very
time consuming process. Earlier specimen preparation was divided in two
categories; for thin films and for bulk materials. Now a days we use
complementary specimen geometry for observations, that of the cross
section, which are made up of layered materials [1]
(a)
(b) (c)
Fig 5- (a) – diffraction pattern from a single crystal (b)- diffraction pattern
from a polycrystalline thin film (c)- diffraction pattern from the same film
with 400 keV kr ion from [1]
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Fig 6- schematic representation of ray paths of scattered and unscattered
rays
Conclusion
All the above explained 'destructive' imaging techniques (SEM, TEM, and
HRTEM), by far are the best techniques for determining the thickness,
structure, and composition of the metal multilayer’s. Despite, having
higher resolution and ability of qualitative analysis, sample preparation for
these techniques is a difficult job in case of metal multilayer’s which
requires precision tools such as diamond saw, metal vapor deposition, FIB,
sophisticated grinding, milling, and polishing equipments and a series of
complex process steps. Longitudinal (surface & structure) and Cross-
sectional (thickness & composition of layers) imaging can be done after
sample preparation.
In case of SEM a small section of the sample is cut and stuck vertically on
a copper support using carbon tape held on to a sample holder which is
then analyzed in SEM using different detectors. Secondary electron
detector is most prominently used which sends all the data to the
computer program to do the computation and generate the image.
Compositional analysis is done in on the sample using the EDAX detector
on the equipment. [1]
For TEM and HRTEM sample preparation is a very critical stage as the
thickness of the sample on the copper grid is limited to a few 100nm
(<<500nm). Sample preparation for TEM involves around 9 complex
process steps and the precision equipments stated above. A very thin
slice is cut through the sample that is then positioned onto the copper
grid and a series of different milling; grinding and polishing steps then
remove all the aberrations and artifacts from the sample surface and also
make it thin enough for the TEM analysis. This a very effective and most
used way of imaging and measuring the thickness of the metal multilayer
and also qualitative analysis is done by studying the difference in contrast
of various metal layers. [1] [2] and [3]
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Bibliography
Books:
[1] Encyclopaedia of material characterization (electronic recourse)
Surfaces, interfaces, thin films Editors: C. Richard Brundle, Charles
A.Evans, and Shaun Wilson part 1-6
1.3.5 page 15, 1.4.1 page 16, 4.1 page 198-200, 1.5.4 page 25, 1.2.4, 2.4
page 99-100, 1.2.2page 8, 2.2page 70-71
Journal articles:
[4] The determination of thin film thickness using reflectance
spectroscopy
Andrew R. Hind PhD and Lisette Chometteb
Varian Limited, 28 Manor Road, Walton-on-Thames, Surrey KT12 2QF,
England
Varian France S.A., 7 Avenue des Tropiques, Z.A. Courtaboeuf 2 - B.P. 12,
91941 Les Ulis, France
Web reference
www.varianinc.com
www.iopscience.iop.org
[7] www.llnl.gov/str/Barbee
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