Studies on Enhancement of Performance of Heat Exchangers Using Nano Particles 2018-19

CHAPTER 1
INTRODUCTION
1.1 Introduction

The Scanning Electron Microscope (SEM) allows visualization of surface features of a

solid sample by scanning through an electron beam. SEM has better resolution capability and
depth of field than a light microscope. As a result of which good quality three dimensional
like images are obtained. In advanced SEM machine, magnification can range from 10× to
5000× and resolution of about 1 nm.
Samples from textile industry, pharmaceutical industry, ceramic industry, polymer industry
and other allied industries can be tested on this SEM.

1.2 Scanning electron microscope

A scanning electron microscope (SEM) is a type of electron microscope that

produces images of a sample by scanning the surface with a focused beam of electrons. The
electrons interact with atoms in the sample, producing various signals that contain
information about the surface topography and composition of the sample. The electron beam
is scanned in a raster scan pattern, and the position of the beam is combined with the intensity
of the detected signal to produce an image. In the most common SEM mode, secondary
electrons emitted by atoms excited by the electron beam are detected using an Everhart-
Thornley detector. The number of secondary electrons that can be detected, and thus the
signal intensity, depends, among other things, on specimen topography. SEM can achieve
resolution better than 1 nanometer.

Figure 1.1 SEM and EDX analysis machine

Department of Mechanical Engineering, Nagarjuna College of Engineering and Technology Bangaloru 1

Studies on Enhancement of Performance of Heat Exchangers Using Nano Particles 2018-19

The Scanning Electron Microscope (SEM) allows visualization of surface features of a

solid sample by scanning through an electron beam. SEM has better resolution capability and
depth of field than a light microscope. As a result of which good quality three dimensional
like images are obtained. In advanced SEM machine, magnification can range from 10× to
5000× and resolution of about 1 nm.
Samples from textile industry, pharmaceutical industry, ceramic industry, polymer industry
and other allied industries can be tested on this SEM.

1.3 Scanning Electron Microscopy (SEM) with Energy Dispersive X-Ray

Analysis (EDX)

SEM provides detailed high resolution images of the sample by rastering a focussed electron
beam across the surface and detecting secondary or backscattered electron signal. An Energy
Dispersive X-Ray Analyzer (EDX or EDA) is also used to provide elemental identification
and quantitative compositional information.

SEM provides images with magnifications up to ~X50,000 allowing sub micron-scale

features to be seen i.e. well beyond the range of optical microscopes.
1. Rapid, high resolution imaging with identification of elements present
2. Spatially resolved quantitative EDX (EDA) analysis of user defined areas on sample
surface
3. Characterization of particulates and defects
4. Examination of grain structure and segregation effects
5. Coating thickness measurement using cross sectional imaging of polished sections.

Typical Applications

1. Characterization of material structures

2. Assessment of reaction interfaces, service environment and degradation mechanisms
3. Characterization of surface defects, stains and residues on metals, glasses, ceramics
and polymers
4. Measurement of the thickness of layered structures, metallized layers, oxide films,
composite materials using cross sectional imaging
5. Particulate and contaminant analysis on and within materials.

Department of Mechanical Engineering, Nagarjuna College of Engineering and Technology Bangaloru 2

Studies on Enhancement of Performance of Heat Exchangers Using Nano Particles 2018-19

Typical Industries using SEM / EDX

1. Aerospace
2. Automotive
3. Materials
4. Minerals
5. Glass, Ceramics and Refractories
6. Healthcare
7. Medical Devices
8. Semiconductors
9. Electronics.

Department of Mechanical Engineering, Nagarjuna College of Engineering and Technology Bangaloru 3

Studies on Enhancement of Performance of Heat Exchangers Using Nano Particles 2018-19

CHAPTER2
LITERATURE REVIEW
Most of the metallic materials functioning at high temperature need to have
oxidation resistance. This resistance can be achieved when the chosen materials develop
through oxidation, an oxide film which acts as a diffusion barrier while keeping a good
adherence. Several studies have shown that the oxide layers as SiO2, Cr2O3, and α-Al2O3
provide a satisfactory protective role, a protection based on the formation of a layer of α-
Al2O3. Al2O3 is the most powerful principle. In this prospect, α-Al2O3 is a very good
candidate. Before reaching the most stable Al2O3 [1].

Alumino-former materials developed transition Al2O3 among which the most

common are γ, δ, and/or θ phases. Nowadays, it is not clear whether the growth of transition
Al2O3 as a first step improves the protective properties of the further formed α-Al2O3 film.
Moreover, one difficulty associated with the understanding of the influence of transition
Al2O3 on the further oxidation resistance concerns the fact that, as mentioned in [2].

The techniques which allow us to detect and characterize transition Al2O3 formed as
thin layers (1 to 3 μm) are scarce and provide ambiguous answers. Indeed, the most common
technique, the XRD, provides patterns for various Al2O3 which are relatively close to each
other. Moreover, it seems that, in many cases, several transition phases can be simultaneously
present [3].
In previous studies, transmission electron microscopy (TEM) was used to probe the
oxidation of either an intermetallic alloy, Fe3Al, or an ODS (oxide dispersion strengthening)
FeCrAl alloy strengthened by very small Y2O3 particles, PM2000 [4].

The formation of transition Al2O3 for various heat treatment conditions was
evidenced and the transition to the α-Al2O3 was studied. The formed oxide scales were
characterized using analysis techniques such as scanning electron microscope (SEM), energy-
dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Fourier transform infrared
spectroscopy (FTIR), and X-ray photoelectron spectroscopy (XPS). The present study aims at
examining whether FTIR and XPS analysis may provide a simple probe to various structural
varieties of Al2O3 for applications of high temperature materials [5].

Department of Mechanical Engineering, Nagarjuna College of Engineering and Technology Bangaloru 4

Studies on Enhancement of Performance of Heat Exchangers Using Nano Particles 2018-19

CHAPTER3

SEM IMAGE ANALYASIS OF USING AL2O3 NANO

PARTICLES
3.1 Sem images

Pure alluminium
oxides

Unwanted particles

Figure 3.1 Scanning Electron Microscope

Figuere 3.1 show a Scanning electron microscope (SEM) image working distance
11200 micron magnification size of particle is 500 microns, increase the image length 1000
microns. The SEM image clearly shows the small alluminium oxide particles and
wasteparticles at micro size to large size.

The sem machine scans in less than 50 microns of a alluminium oxide particles in a
analysis of the detailed configurations of particular sized particles as shown in the above
image . the sem image shows number of percentage cantains pure aluminum particles present
in the tatol material of the unwanted materials like dust, oxidation particles and other
compound materials found in the testing materials as present in the figure 3.1.

Department of Mechanical Engineering, Nagarjuna College of Engineering and Technology Bangaloru 5

Studies on Enhancement of Performance of Heat Exchangers Using Nano Particles 2018-19

Figure 3.2 Scanning Electron Microscope

Figure 3.2 shows a Scanning electron microscope (SEM) image working distance
11200 micron, magnification size of particle is 400 microns, image size is ( length and width)
is 1000*1000 microns. The SEM image clearly shows the alluminium oxide particles at
micro size to large size.

The sem machine scans in less than 50 microns of a alluminium oxide particles in
a analysis of the detailed configurations of particular sized particles as shown in the above
image . the sem image shows number of percentage cantains pure aluminum particles present
in the tatol material of the unwanted materials like dust, oxidation particles and other
compound materials found in the testing materials as present in the figure 3.2.

Department of Mechanical Engineering, Nagarjuna College of Engineering and Technology Bangaloru 6

Studies on Enhancement of Performance of Heat Exchangers Using Nano Particles 2018-19

Figure 3.3 Scanning Electron Microscope

Figure 3.3 shows a Scanning electron microscope (SEM) image working distance
11200 micron, magnification size of particle is 200 microns, image size is ( length and width)
is 2000*2000 microns. The SEM image clearly shows the single alluminium oxide particles
at micro size to large size.

The sem machine scans in less than 50 microns of a alluminium oxide particles in a
analysis of the detailed configurations of particular sized particles as shown in the above
image . the sem image shows number of percentage cantains pure aluminum particles present
in the tatol material of the unwanted materials like dust, oxidation particles and other
compound materials found in the testing materials as present in the figure 3.3.

Department of Mechanical Engineering, Nagarjuna College of Engineering and Technology Bangaloru 7

Studies on Enhancement of Performance of Heat Exchangers Using Nano Particles 2018-19

Figure 3.4 Scanning Electron Microscope

Figure 3.4 shows a Scanning electron microscope (SEM) imag working distance
11200 micron, magnification size of particle is 950 microns, image size is ( length and width)
is 5000*5000 microns. The SEM image clearly shows the alluminium oxide particles at
micro size to large size.

The sem machine scans in less than 50 microns of a alluminium oxide particles in a
analysis of the detailed configurations of particular sized particles as shown in the above
image . the sem image shows number of percentage cantains pure aluminum particles present
in the tatol material of the unwanted materials like dust, oxidation particles and other
compound materials found in the testing materials as present in the figure 3.4.

Department of Mechanical Engineering, Nagarjuna College of Engineering and Technology Bangaloru 8

Studies on Enhancement of Performance of Heat Exchangers Using Nano Particles 2018-19

Figure 3.5 Scanning Electron Microscope

Figure 3.5 shows a Scanning electron microscope (SEM) image working distance
11200 micron, magnification size of particle is 500 microns, image size is ( length and width)
is 10000*10000 microns. The SEM image clearly shows the alluminium oxide particles at
micro size to large size

The sem machine scans in less than 50 microns of a alluminium oxide particles in
a analysis of the detailed configurations of particular sized particles as shown in the above
image . the sem image shows number of percentage cantains pure aluminum particles present
in the tatol material of the unwanted materials like dust, oxidation particles and other
compound materials found in the testing materials as present in the figure 3.5.

Department of Mechanical Engineering, Nagarjuna College of Engineering and Technology Bangaloru 9

Studies on Enhancement of Performance of Heat Exchangers Using Nano Particles 2018-19

Figure 3.6 Scanning Electron Microscope

Figure 3.6 shows a Scanning electron microscope (SEM) image working distance
11200 micron, magnification size of particle is 250 microns, image size is ( length and width)
is 20000*20000 microns. The SEM image clearly shows the number of alluminium oxide
particles at micro size to large size.

The sem machine scans in less than 50 microns of a alluminium oxide particles in a
analysis of the detailed configurations of particular sized particles as shown in the above
image . the sem image shows number of percentage cantains pure aluminum particles present
in the tatol material of the unwanted materials like dust, oxidation particles and other
compound materials found in the testing materials as present in the figure 3.6.

Department of Mechanical Engineering, Nagarjuna College of Engineering and Technology Bangaloru 10

Studies on Enhancement of Performance of Heat Exchangers Using Nano Particles 2018-19

Figure 3.7 Scanning Electron Microscope

Figure 3.7 shows a Scanning electron microscope (SEM) image working distance
11200 micron, magnification size of particle is 100 microns, image size is ( length and width)
is 50000*50000 microns. The SEM image clearly shows the number of clean alluminium
oxide particles shows at micro size to large size.

The sem machine scans in less than 50 microns of a alluminium oxide particles in a
analysis of the detailed configurations of particular sized particles as shown in the above
image . the sem image shows number of percentage cantains pure aluminum particles present
in the tatol material of the unwanted materials like dust, oxidation particles and other
compound materials found in the testing materials as present in the figure 3.7.

Department of Mechanical Engineering, Nagarjuna College of Engineering and Technology Bangaloru 11

Studies on Enhancement of Performance of Heat Exchangers Using Nano Particles 2018-19

3.2 ENERGY DISPERSIVE X-RAY SPECTROSCOPY ( EDX)

The figure 3.8 and graphs are shows the percentage of carbon,oxygen and pure
alluminium present at raw material of alluminium oxide.

Figure 3.8 Energy dispersive X-ray spectroscopy image.

Image Name: Base(342)(94)

Image Resolution: 512 by 384
Image Pixel Size: 0.00 µm
Acce. Voltage:13.0 kV
Magnification of image: 4000

EDX AND SEM provides detailed high resolution images of the sample by rastering
a focussed electron beam across the surface and detecting secondary or backscattered electron
signal. An Energy Dispersive X-Ray Analyzer (EDX or EDA) is also used to provide
elemental identification and quantitative compositional information.

Department of Mechanical Engineering, Nagarjuna College of Engineering and Technology Bangaloru 12

Studies on Enhancement of Performance of Heat Exchangers Using Nano Particles 2018-19

The above graph shows the plot the graph x-axis and y-axis in x-axis the current in
volts and y-axis log scale and mid point is base line of the graph. So that in the graph the
percentage of carbon,oxidation and pure alluminium oxide present it. It is clearly shows the
three elements of metals are present in the different ratios of percentages indiacates the as
shown in the graph.

Department of Mechanical Engineering, Nagarjuna College of Engineering and Technology Bangaloru 13

Studies on Enhancement of Performance of Heat Exchangers Using Nano Particles 2018-19

Department of Mechanical Engineering, Nagarjuna College of Engineering and Technology Bangaloru 14

Studies on Enhancement of Performance of Heat Exchangers Using Nano Particles 2018-19

C-K O-K Al-K

Base(342)(94)_pt1 0.79 39.46 59.74
Base(342)(94)_pt2 27.70 72.30
Base(342)(94)_pt3 18.31 81.69

Weight % Error (+/- 1 Sigma)

C-K O-K Al-K
Base(342)(94)_pt1 ±0.30 ±1.12 ±1.48
Base(342)(94)_pt2 ±1.26 ±1.99
Base(342)(94)_pt3 ±1.24 ±2.64

Atom %
C-K O-K Al-K
Base(342)(94)_pt1 1.39 51.96 46.65
Base(342)(94)_pt2 39.25 60.75
Base(342)(94)_pt3 27.43 72.57

Atom % Error (+/- 1 Sigma)

C-K O-K Al-K
Base(342)(94)_pt1 ±0.52 ±1.47 ±1.16
Base(342)(94)_pt2 ±1.78 ±1.67
Base(342)(94)_pt3 ±1.86 ±2.34

Department of Mechanical Engineering, Nagarjuna College of Engineering and Technology Bangaloru 15

Studies on Enhancement of Performance of Heat Exchangers Using Nano Particles 2018-19

CONCLUSIONS
The aim of this work was to determine whether IR spectroscopy and XPS could allow us to
easily distinguish the different structural varieties of Al2O3 and therefore be used as a rapid
diagnostics to evidence the phases present in the protective layers of high temperature
materials. It was thus possible to determine the FTIR spectra of Al2O3 phases and the XPS
analysis at different temperatures of oxidation and to evidence a continuous evolution leading
to the simultaneous presence of several Al2O3 phases. These results have allowed us to
determine some characteristic IR and XPS peaks, that is, signatures, for the various transition
Al2O3 phases and α-Al2O3. Using these IR and XPS signatures, it is possible to detect the
presence of transition Al2O3 naturally grown on Al2O3-former alloys. A detailed example is
presented for the oxidation of PM2000 ODS alloy. Indeed, many high temperature metallic
materials develop Al2O3 scales that can act as protective layer against an aggressive
environment. In the first stage, mixed Fe, Cr oxides, and transition Al2O3 appear; afterwards
Al2O3 oxides become gradually the majority as the oxidation temperature increases before
transformation into the most stable α-Al2O3 structure. Although the physical properties of the
transition Al2O3 differ, their identification is not straightforward.

Department of Mechanical Engineering, Nagarjuna College of Engineering and Technology Bangaloru 16

Studies on Enhancement of Performance of Heat Exchangers Using Nano Particles 2018-19

FUTURE SCOPE
We want to mention that the measurements such as high temperature dc magnetization and
mossbaucer spectroscopy will provide us information about magnetic ordering in these
materials near and above the neel temperature. The dielectric and magnetic properties of Al
doped Ni-Cd ferrite nanoparticles suggest that these materials are very good for the
manufacturing of multi layer inducator chips (MLICS),high density data storage devices.The
important size dependent superparamagnetic properties of Ni0.2,Cd0.3,Fe2.5-xAlxO4
nanoparticles unambiguously make Ni0.2,Cd0.3,Fe2.5-xAlxO4 as promising candidates for
various practical applications such as MRI contrast enhancement agents ,magnetic probes for
biomolecules and magnetically guided drug delivery.

Department of Mechanical Engineering, Nagarjuna College of Engineering and Technology Bangaloru 17

Studies on Enhancement of Performance of Heat Exchangers Using Nano Particles 2018-19

REFERENCES
[1]. R. Molins and A. M. Huntz, “Recent improvements in the understanding of alumina film
formation and durability,” Materials Science Forum, 461–464, 29–36, 2004.

[2]. S. Chevalier, R. Molins, O. Heintz, and J. P. Larpin, “Which tool to distinguish transient
alumina from alpha alumina in thermally grown alumina scales?” Materials at High
Temperatures, 22, 527–534, 2005.

[3]. H. El Kadiri, R. Molins, Y. Bienvenu, and M. F. Horstemeyer, “Abnormal high growth

rates of metastable Al2O3 on FeCrAl alloys,” Oxidation of Metals, 64, 63–97, 2005.

[4]. A. M. Huntz, P. Y. Hou, and R. Molins, “Study by deflection of the oxygen pressure
influence on the phase transformation in Al2O3 thin films formed by oxidation of Fe3Al,”
Materials Science and Engineering A,467, 59–70, 2007.

[5]. L. Maréchal, B. Lesage, A. M. Huntz, and R. Molins, “Oxidation behavior of ODS Fe-
Cr-Al alloys: aluminum depletion and lifetime,” Oxidation of Metals, 60, 1–28, 2003.

[6]. M. H. Heinonen, K. Kokko, M. P. J. Punkkinen, E. Nurmi, J. Kollár, and L. Vitos,

“Initial oxidation of Fe–Al and Fe–Cr–Al alloys: Cr as an Al2O3 Booster,” Oxidation of
Metals, 76, 331–346, 2011.

[7]. A. H. Heuer, T. Nakagawa, M. Z. Azar et al., “On the growth of Al2O3 scales,” Acta
Materialia, 61, 6670–6683, 2013.

[8]. M. F. López, A. Gutiéerrez, M. C. García-Alonso, and M. L. Escudero, “Surface analysis

of a heat-treated, Al-containing, Fe-based superalloy,” Journal of Materials Research, 13,
3411–3416, 1998.

[9]. J. Engkvist, U. Bexell, T. M. Grehk, and M. Olsson, “ToF-SIMS depth profiling of

alumina scales formed on a FeCrAl high-temperature alloy,” Applied Surface Science, 231-
232, 850–853, 2004.

[10]. D. Naumenko, W. J. Quadakkers, A. Galerie, Y. Wouters, and S. Jourdain, “Parameters

affecting transient oxide formation on FeCrAl based foil and fibre materials,” Materials at
High Temperatures, 20, 287–293, 2003.

Department of Mechanical Engineering, Nagarjuna College of Engineering and Technology Bangaloru 18