Preparation and Characterization of Nanoparticles for use in Efficient

Heat Transfer.

Mini Project Report Submitted to

Shivaji University, Kolhapur

For the Degree of

Bachelor of Technology

in

Chemical Technology

Under the Faculty of Engineering & Technology

By

Ms. Mahajan Saie H.

Mr. Shejul Hrishikesh D.

Mr. Yadav Tushar R.

Mr. Sawant Sangram V.

Under the Guidance of

Mr. Rao A. S.
DEPARTMENT OF TECHNOLOGY,
SHIVAJI UNIVERSITY, KOLHAPUR

Year: 2017-18
 DECLARATION

We hereby declare that the Mini Project report entitled, ‘Preparation and
Characterization of Nanoparticles for use in Efficient Heat Transfer.’ has
been completed and written by us for the award of degree of Bachelor of
Technology in Chemical Technology. The contents of this report are
written by us and are not copied from any source or published anywhere
in any form prior to the submission, for the award of any graduate
course.

Ms. Mahajan Saie H.

Mr. Shejul Hrishikesh D.

Mr. Yadav Tushar R.

Mr. Sawant Sangram V.

Date:

Place:
 CERTIFICATE

This is to certify that the Mini Project work entitled ‘Preparation and
Characterization of Nanoparticles for use in Efficient Heat Transfer.’ has
assessed by us and found to be completed in all aspects for fulfillment of
work to be done under Mini Project head of Final Year B.Tech
(Chemical Technology) which is being submitted herewith for the award
of degree of ‘Bachelor of Technology’ in Chemical Technology of
Shivaji University, Kolhapur. It is the result of the work completed by
Ms. Mahajan Saie H.

Mr. Shejul Hrishikesh D.

Mr. Yadav Tushar R.

Mr. Sawant Sangram V.

Project Guide Program Coordinator

Date:

Place:
MINI PROJECT TITLE- Preparation and Characterization of
Nanoparticles for use in Efficient Heat Transfer.

ATTAINMENT OF COURSE OUTCOMES

CO statements Attainment levels

Low Medium High
1 Identify social, environmental, market needs and
solutions.
2 Understand design and development stages in
electronics engineering projects.
3 Apply engineering knowledge for solving real world
problems.
4 Manage project and finance.
5 Provide technological solutions on recent problems
and lifelong learning.
6 Work in team, follow ethical practices, and prepare
documentation and presentation.

Student signatures

1]

2]

3]

Project Guide Program Coordinator

B.Tech.(Chemical Technology)
 ATTAINMENT OF PROGRAM OUTCOMES
PO PO Statements Attainment levels
No. Excellent Very good Good Average Poor
1 Domain specific Engineering knowledge : Attainment of the ability to acquire and apply
knowledge of mathematics, physics, chemistry, basic engineering sciences and Chemical
Engineering specialization so as to make analysis of complex chemical engineering problems.
2 Problem Analysis ability: Attainment of the ability to acquire knowledge which will enable
them to analyze problems while working in chemical and allied industries as well as
consultancies.
3 Acquiring skills to Design/develop solutions to problems: Acquiring skills in selection, design,
erection and control of unit processes and unit operations and to attain ability to understand
the past and present trends in manufacturing, production and marketing of chemically
derived products.
4 Capacity to investigate complex problems : Attainment of the ability to identify new research
areas in chemical engineering and to use research based knowledge and research methods
including design of experiments, analysis and interpretation of data, and synthesis of the
information to provide valid conclusions, also to make efforts to come up with striking
innovations in the field.
5 Modern tool usage: Attainment of the ability to create, select and apply appropriate
techniques, resources, and modern engineering and IT tools including ‘modeling and
prediction’ to complex engineering activities so as to solve advanced engineering problems.
6 The engineer’s connectivity with society: Apply reasoning informed by the contextual
knowledge to assess societal, health, safety, legal and cultural issues and the consequent
responsibilities relevant to the professional engineering practice.
7 Environment and sustainability awareness: Understand the impact of the professional
engineering solutions in societal and environmental contexts, and demonstrate the
knowledge of, and need for sustainable development.
8 Practicing Ethics and Values: Apply ethical principles and commit to professional ethics and
responsibilities and norms of the engineering practice.
9 Ability to work as an Individual and in team: Function effectively as an individual, and as a
member or leader in diverse teams, and in multidisciplinary settings.
10 Acquiring Communication Skills: Communicate effectively on complex engineering activities
with the engineering community and with society at large, such as, being able to
comprehend and write effective reports and design documentation, make effective
 presentations, and give and receive clear instructions.
11 Well verse with task of Project management and finance aspects: Demonstrate knowledge
and understanding of the engineering and management principles and apply these to one’s
own work, as a member and leader in a team, to manage projects and in multidisciplinary
environments.
12 Life-long learning attitude: Recognize the need for, and have the preparation and ability to
engage in independent and life-long learning in the broadest context of technological
change.
PSO PSO Statements
No.
1 1. Professional skills : Acquiring skills to utilize the knowledge of chemical engineering in
innovative, dynamic and challenging environment for design and development of new
products, attainment of ability to acquire skills required to help chemical industry through
courses like Process Design , Piping Design and the relevant software training

2 2. Practical implementation and testing skills: Attainment of ability to acquire skills required to
help chemical industry. These may be imbibed through courses/workshops on industrial
safety & hazard management, hands on training for topics like ‘analytical techniques’,
‘instrumentation’ required in chemical and allied industry.

3 3. Successful career and entrepreneurship: Transformation of the students into technocrats

who will design and develop systems and subsystems for Chemical allied Technologies and
few of these technocrats may become entrepreneurs also.

Student signatures
1]
2]
3] External Examiner Project Guide Program Co-ordinator
ACKNOWLEDGEMENT
 LIST OF FIGURES
Chapter Figure No. Figure name Page No.
No.
7 1 Solution after 40 mins
7 2 Solution after 1 hour
8 3 FTIR data of CuO Nanoparticles
8 4 Photoluminescence spectrum of CuO
Nanoparticles
8 5 XRD of CuO Nanoparticles
8 6 UV – vis – NIR Spectroscopy
 LIST OF TABLES
Chapter Table No. Table name Page No.
No.
3 1 Materials and their Thermal Conductivity
7 2 Time vs Temp./ pH while preparation
 INDEX
Chapter Name of Chapter Page numbers
No.

1 TITLE 01-05

2 OBJECTIVE 06-10

3 METHODOLOGY

4 APPARATUS USED

5 CHEMICALS USED

6 INSTRUMENTS USED

7 THEORY

8 EXPERIMENTAL SETUP AND

PROCESS

9 MEASUREMENTS AND
FINDINGS

10 ECONOMICS

11 CONCLUSION

12 RECOMMENDATION

13 FUTURE SCOPE

14 BIBLIOGRAPHY
 Preparation and Characterisation of Nanoparticles
for use in Efficient Heat Transfer.

2. Objective:
To synthesize CuONanoparticles and analyze its characteristic properties for it's
further use inefficientHeat Transfer.

3. Methodology:
3.1) Introduction – Heat Transfer is one of the most important industrial
process with progress of thermal science and engineering, it has been of a strong
interest to develop micro scale liquid flow device, which have compactness and
high surface to volume ratio compared to conventional fluids. An efficient way of
improving thermal conductivity of fluids in order to change the transport
potencies, flow and heat transfer features.
It has been known that micro or millimetre sized solid particles added into
a base fluid can improve the thermal conductivity of the fluid. Although they may
improve heat transfer coefficient of the fluids, they practical applications limited
because of sedimentation of particles, clogging flow channels, erosion of pipelines
and causing pressure drops
Nanofluids, which are solid liquid composite materials composing of a
nanometre sized solid particles fibres, rods or tubes suspended in gas besides
anomalously high thermal conductivity. Nanofluids represent improved stability
compared with conventional fluids added with micro or millimetre sized solid
particles because of size effect ad Brownian motion of the fluids in liquids. With
such ultrafine Nanoparticles, NF’s can flow smoothly in a micro channel and the
size of the use of NF with high heat efficiency.
In this report we shall discuss about the preparation and properties,
characterisation of Nanoparticles for such purposes and the following aspects
involved.
 Availability of Nanoparticles.
 Selection of Nanoparticles.
 Characterisation of Nanoparticles.

3.2) Availability of Nanoparticles:

While selecting this topic as our Mini Project we first reviewed literature and
marked the processes for Synthesis of Nanoparticles that were possible at our
institute level. We found out that Nanoparticles of Cu and Al were most readily
available.
3.3) Selection of Nanoparticles:
Theoretically all solid Nanoparticles with high thermal conductivity can be used
as additives of NF’s. Nanoparticles often used to prepare NF’s are:
a. Metallic particles (Cu, Al, Fe, Au and Ag)
b. Non-Metallic particles (Al2O3, CuO, Fe3O4, TiO2, SiC)
c. Carbon Nanotubes.
The base fluids used as water, ethylene glycol, acetone, oil.

Materials Thermal Conductivity (W/mK)

Metallic Solids Cu 401
Al 237
Ag 428
Au 318
Fe 83.5
Non Metallic CuO 76.5
Solids Al2O3 83.5
SiC 148
Base Fluids H2O 0.613
EG 0.253
Table 1.Materials and their Thermal Conductivity.

3.4) Synthesis of Nanoparticles:

Chemical Precipitation is prominent technique for the synthesis of Nanoparticles.
In this method Copper salt is used in the presence of Sodium Hydroxide,
Deionised double distilled water was used throughout the experiment.
The synthesized Nanoparticles are characterised for X-Ray diffraction (XRD)
studies, Scanning Electron Microscopy (SEM) analysis for their size and shapes.
The sizes of the synthesized Nanoparticles are in nano scale. With spherical
structures irrespective of the technique used. Band gap energy was evaluated for
all the synthesized samples from UV visible Spectrophotometer analysis.
4. Apparatus Used:
Apparatus used for Synthesis of CuO Nanoparticles:
1. Magnetic Stirrer.
2. Hot Air Oven.
3. Filter Paper.
4. pH meter.
5. pH paper.

5. Chemicals Used:
1. Deionised Water.
2. Copper Chloride dihydrate.
3. Sodium Hydroxide.
4. Hydrochloric Acid.

6. Instruments for Characterisation:

1. UV – Visible – NIR – DRS Spectrophotometer V770, Jasco, Japan.
(Spectroscopy)
2. FTIR Spectrometer 4600, Jasco, Japan. (Infrared spectrum)
3. Spectrofluorometer FP8200, Jasco, Japan. (Fluorescence)
4. X – Ray Diffraction D8 Discover Instrument, Burke.

7. Theory:
Copper oxide nanofluid has been prepared using wetchemical method. All
the chemicals such as copper chloride, sodium hydroxide, and hydrochloric acid
were availablein the laboratories and they are in analyticalgrade. Since the method
involves single-step process, thepreparation of copper oxide nanoparticle is
carried out by a simple yet precise technique.
In this preparation process, 100 ml ofdeionised water is taken in a 500 ml
of beaker. To this 0.51g of copper chloride was added along with 1 gram
ofsodium hydroxide pellets. The reaction mixture was heated along with magnetic
stirring and the process is carried out for one hour. The rpm for magnetic stirring
was set at 200 and temperature was maintained at 60°C. As a result, the color of
the solution changes from blue to black after the reaction, and then the mixture
was cooled to room temperature. While the process was going on the pH was
maintained at near 11.
Schematically the chemical reaction can be represented as:
CuCl2 + 2NaOH = CuO + NaCl + H2O.
The pH value of the so formed copper oxide wet precipitate is neutralized by
adding droplets of hydrochloric acid. For this particular sample we needed total
2.1 ml of HCl which was added drop by drop measuring the pH at every drop.
Then the copper oxide wet precipitate is washed with deionised water to remove
the impurity ions present in the solution.

Fig.1. Solution after 40 mins.

Fig. 2. Solution after 1 hour.

 70

60

50

40

30
Temperature
20 pH
10

0
0 10 20 30 40 50 60
Time (min)

Table 2. Time vs Temp./ pH while preparation

8. Experimental Setup and Process:

A. Physio – Chemical Characterisation
1. Scanning Electron Microscope (SEM): Analysis was carried
out to study to study the morphology of Nanoparticles for SEM analysis 0.1 gm
sample was used of CuO.
2. X-Ray Diffraction (XRD): To identify the crystal structure of
Nanoparticles X-Rays powder diffraction (XRD) was performed.
3. UV-vis-NIR-Spectroscopy: Several methods can be applied o
characterize the optional properties and to obtain the band gap UV-visible
spectroscopy is one of the methods for determining the band gap of CuO
Nanoparticles. It is used for evaluating the optical absorption characteristic of
CuO Nanoparticles.
4. Fourier Transform Infrared (FTIR): The synthesized
sample was analysed with FTIR spectrometry. During this process, a small
amount of powder was transferred into a sample cup of the diffuse reflectance
accessory and scanned in a region of about 400 – 500 cm-1. FTIR was particularly
used for determining the presence of any residual functional groups present in
Nanoparticles.
 5. Brunauer-Emmett-Teller Surface Area: This Surface area
test shows, as the name suggests, the surface area of the particle and also the
porosity of the particle. This is essential if we want to use the Nanoparticles for
Heat Transfer.
6. Fluorescence Test: This is small test which confirms the
presence of Copper Oxide material in the prepared sample as CuO particles are
known to show Fluorescence under right wavelength of light.

9. Measurements and Findings:

By Conducting the above mentioned tests the following were the results:

9.1) FT-IR (Fourier Transform Infrared)

Figure 3.FTIR data of CuO Nanoparticles.

The FT-IR spectrum used to characterize the functional groups of the CuO
nanoparticles was carried out in the range 399 – 7800 cm-1. The instrument used
was FTIR - 4600. The spectrum depicts vibrational modes in range 3000 - 4000
cm-1 which are related to the vibrations of Hydrogen bonds present. The
characteristic bands of copper oxide, at 615 and 502 cm-1 are clearly visible and
have a high intensity. The band positioned at around 615 cm-1 is due to Cu-O
stretching along the direction in agreement with earlier data reported [7-9] and
that at 480 cm-1 is assigned to the Cu-O stretching along of the direction. The
other bands observed in the spectrum are of relatively low intensity, the band at
2923 cm-1 is assigned to the presence of atmosphericCO2 or a Hydrocarbon
Bond.

9.2) Photoluminescence (Fluoresence Test):

Figure 4.Photoluminescence spectrum of CuO Nanoparticles.

The photoluminescence spectrum, at room temperature of prepared CuO

nanoparticles, is shown in Figure 2 after excitation with a wavelength of 580 nm.
It covers the entire visible range with two distinct bands centred at 570 and 590
nm. Various factors are often involved in setting up the photoluminescence
spectrum of a given material. In the visible range, PL emission is mainly
attributed to the presence of defects like vacancies or impurities of materials. For
the copper oxide CuO, vacancies may belong to copper or oxygen while the
impurities may be interstitial copper or anti-oxygen sites CuO.These defects
 induce the formation of new energy levels in the band gap and, as a result,
emissions will arise from these trapped levels during excitation of the sample.
Emission occurs due to radiative recombination of a photo-excited hole with an
electron and the emission bands are commonly referred to as deep level or trap
site emission due to oxygen vacancies.

9.3) XRD:

XRD
16000
14000
12000
Intensity (au)

10000
8000
6000
4000
2000
0
53.2828

64.1031

74.9234

85.7437
10.00161
12.16567
14.32973
16.49379
18.65785
20.82191
22.98597
25.15003
27.31409
29.47815
31.64221
33.80627
35.97033
38.13439
40.29845
42.46251
44.62657
46.79063
48.95469
51.11875

55.44686
57.61092
59.77498
61.93904

66.26716
68.43122
70.59528
72.75934

77.08746
79.25152
81.41558
83.57964

87.90776
Angle ( 2 Theta)

Figure 5.XRD of CuO Nanoparticles.

XRD pattern of as prepared CuO nanoparticles is shown in figure 3. The

intensities and positions of observed diffraction peaks are in good agreement with
the reported values in the JCPDS files. It indicates that we have a single-phase
with monoclinic structure. The good resolution of the main diffraction peaks
reflects the good crystallization of the CuO particles. The sizes of CuO crystallites
are estimated using formula of Debye-Scherrer: = D = 0.9 λ/βcosθ where λ is the
wavelength of X-Ray, β is the FWHM (full width at half maximum) of diffraction
peak, θ is the diffraction angle and D is the size of particles. The average
crystallite size is found in the range 70.23 – 85.76 nm
9.4) UV-vis-NIR-Spectroscopy:

Figure 6. UV – vis – NIR Spectroscopy.

The absorption edge is found so that the type of transition and bandgap value can
be determined. The absorption spectra were used to study the energy band and the
type of electronic transitions. Absorption spectra of CuO nanoparticles are shown
in Fig. 4, which show a strong fundamental absorption edge approximately 292
nm due to direct transition of electrons. Optical absorption shows that the direct
band gap compared to indirect band gap permits us to determine the crystallinity
of a material.

10. Economics:
10.1) Applications of Nanoparticles:
a. Nanoparticles can be used to generate steam without actually
boiling the water, hence saving the energy that goes into boiling the water.
 b. Cooling is one of the most essential scientific challenges in
different industries. Nanofluids can be used in transport systems such as
automotive and automobile radiators and in metal processing they are used in
metal cutting.
c. They could be used as efficient coolants in data centres and
electronic cooling systems. Nanoparticles are used in solar absorption cooling
systems where the particles enhance the absorption property of the conventional
working fluid in solar energy.
d. Other Non- chemical related applications include and extend to
use as Catalyst, Superconducting Materials, Thermoelectric materials, sensing
materials, glass ceramics and other fluids.
e. Nanoparticles are also used as ceramic resistors, Magnetic
storage, Media for gas sensors, IR tilters, photoconductive and Photo thermal
applications.
f. The most significant application ,which we are going to pursue is
in Heat Transfer. In addition to the first and second point, Nanoparticles when
added to Nanofluids and then used as Heat transfer media is very economical and
energy saving. Due to the presence of Nanoparticles in the fluid, the surface area
of the fluid increases, thereby increasing the Heat transfer efficiency.

Talking about the economical aspects, addition of Nanoparticles to the HT

medium increases the efficiency up to 20 – 25% as compared to ordinary fluids.
In layman’s terms, only 75-85% of materials or energy is needed for the
Nanofluids to perform the same task performed by Ordinary fluids.
As mentioned previously, only a fraction of Nanoparticles are added to the base
fluids to make it into Nanofluids. As of now the prices for CuO Nanoparticles in
market is around ₹ 2500/kg. For example, If we consider the volume fraction of
Nanoparticles for preparing Nanofluids to be 4.5%. Then we can prepare about 20
tonnes of Nanofluid which will replace ordinary fluid in Heat Transfer operation.
It is to be noted that this is just a primary observation which needs to be exploited
further. We will discuss the problems that might pose for this method in
Recommendations.

11. Conclusion:
Cuo Nanoparticles were synthesized by Precipitation method and various tests for
confirmation and for finding the various properties of the said Nanoparticles were
performed. Diffraction test revealed that the Material we synthesized was actually
Nanoparticles. Structural, Chemical and Electrical properties of CuO
nanoparticles were studied using XRD, Photoluminescence, FTIR, BET Surface
area test, UV Spectroscopy.
While Preparation or Synthesis of the Particles we concluded that maintaining the
purity of the sample to be produced was of the utmost importance. At first few
attempts, the data was not recorded properly and hence we got unwanted and
anomalous results. The main issue with the preparation was maintaining the
temperature. But as shown in Table 2, It was remedied immediately and
satisfactory results were obtained.
The second challenge we faced while preparation was neutralizing the precipitate
after formation. During the literature review, we found no exact detail as to how
the solution was to be neutralized. It was remedied by continuously measuring the
pH while adding HCl in the solution.
While analysing the test results we concluded that Monoclinic crystalline phase
was obtained of CuO from the XRD analysis. The analysis by FTIR spectroscopy
showed the presence of Cu-O vibration modes and so confirms the result of XRD
analysis on formation of CuO. From thePhotoluminescence test spectra we find
the intensity of emission and emission peak wavelength changes.

12. Recommendations:
Research for Nanoparticles and Nanofluids is in primal stage in field of Chemical
and Biological fields. Although the results for usage of nanoparticles are
promising in these fields, more advanced and thorough research is needed for its
proper applications.
Purity of the Nanoparticles that were synthesized in the institute’s laboratory was
certainly not up to the mark. Hence, more precautions and precise instruments are
needed for more pure and accurate results.
Adding to what discussed in Economics section, the biggest problem for creating
Nanofluids at such large scale will be a far greater problem than at Lab scale. The
second difficulty will be maintaining the purity of the product. Hence to counter
these problems, research on literally large scale need to be done and not just on
laboratory scale.

13. Future Scope:

Nanoparticles have great potential of becoming the next big breakthrough in the
world. Just more people are needed to be encouraged for researching in this field.
Not only in Chemical field, but biology has a lot of application for Nanoparticles
and Nanofluids as well such as Nano drug delivery system, etc.
It has the potential of replacing Conventional fluids used in Heat transfer i.e.
Water which in turn converts to steam. Hence Nanofluids, if the research process
is a success and economically feasible, can be the base fluids for every Heat
Transfer Operation.
The next step at our level will be checking and testing its potential of CuO
Nanoparticles when they are converted to Nanofluids and how they affect the
Heat transfer efficiency and Thermal conductivity of the Base fluids.

14. Bibliography:
1. R. Manimaran, K. Palaniradja, N. Alagumurthi, S. Sendhilnathan, J. Hussain
(2012) - Preparation and characterization of copper oxide nanofluid for heat
transfer applications. Appl. Nanosci 4:163-167.
2. N C Horti , M. D. Kamatagi, S. K. Nataraj -Photoluminescence Properties of
Copper Oxide nanoparticles.
3. B Troudi, O. Halimi, M. Sebais, B. Boudine, A. Djebli (2016) - Synthesis,
Strucutural and Optical properties of CuO Nanocrstyals . WIC 69-73.
4. A. Radhakrishnan, B. Beena (2014) – Structural and Optical Absorption of
CuO Nanoparticles. IJACS 2: 158-161
5.