CHAPTER 1

INTRODUCTION

1.1 GENERAL

Storage of thermal energy becomes an important aspect of engineering

application, especially in energy conservation in buildings. Along with that due to the
increase in energy demand globally and the increasing levels of greenhouse gases,
researchers are continuously looking for greener alternatives for energy storage and
supply. Over the past few decades, the rapid growth of fossil energy consumption
caused by the great development of population and economy has resulted in severe
environmental pollution and global warming. The increasing energy consumption will
result in several energy problems such as supply difficulties, exhaustion of energy
resources, climate change, and environmental pollution. There are various thermal
energy storage methods, but latent heat storage is the most used one due to high
storage density and small temperature variation from storage to retrieval. In a latent
heat storage system, energy is stored during melting and recovered during the freezing
of a phase change material (PCM).

1.2 PHASE CHANGE MATERIALS

Phase change materials are an upcoming trend to reduce energy consumption in

a wide range of applications. It can reduce the high energy consumption of the
building and it can provide a high energy storage density with the change between the
solid phase and liquid phase and thus reducing the temperature fluctuations inside
buildings. only solid to liquid and liquid to solid phase change transition are applicable
for PCMs. comparing to conventional storage materials such as water, masonry or
rock, PCM can store up to 5 to 14 times more heat per unit volume.

Phase change materials (PCMs) absorb or release latent heat through phase
transformation, reducing temperature swings as well as decreasing the mismatch
between energy supply and energy consumption which are very effective in storing
latent heat and improving energy utilization efficiency. The incorporation of phase
change material into the construction materials can decrease the heating and cooling

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demand of the building.From the investigation of Phase change materials (PCMs),
fatty acids like lauric acid and palmatic acid act as thermal energy storage devices.

1.3 CLASSIFICATION OF PCM

The main categorization of PCMs is the differentiation between inorganic PCMs

and organic PCMs. The commonly used phase-change substances for technical
applications are as follows: paraffins (organic), fatty acids (organic), and salt hydrates
(inorganic). Fig. 1.5 shows the relationship between PCM’s enthalpy and temperature
for different types of PCMs. These characteristics are especially important for their
application in building envelopes since PCM has to be incorporated into the structural
components, finish materials, or thermal insulation. A very common situation is when
for a specific application, there is no single PCM product that possesses all the
required properties and performance characteristics. In such circumstances, the overall
design of the PCM system has to be modified to make up for the missing physical
properties.
1.3.1 ORGANIC COMPOUNDS
These are organic materials and further sub-categorizedas paraffins and non-
paraffins.
1. Paraffins:
These are mostly straight chain alkanes. Their melting point and latent heat
increase with increase in chain length.

Advantages:
 Availability in large temperature range.
 Congruent melting and good nucleating properties.
 Reliable and predictable behaviour.
 Safe and non- corrosive.
 Economic.
Disadvantages:
 Low thermal conductivity
 Non-compatibility with plastic containers.
 Moderately flammable.

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2. Non-paraffins:
These are most numerous PCMs with varied properties. Most of them are esters,
fatty acids, alcohols and glycols with high heat of fusion.
Advantages:
 High heat of fusion.
 Inflammable.
Disadvantages:
 Low thermal conductivity.
 Low flashpoint.
 Instability at higher temperature.

1.3.2 INORGANIC COMPOUNDS

Inorganic PCMs are further categorized as salt hydrates and metallics. These PCMs do
not show appreciable super cooling and show favourable thermal cycling.
a. Salt hydrates:
These are nothing but the alloys of inorganic salt and water, in which crystalline solids
are formed. Solid-liquid phase transition of salt hydrates is the process of hydration
and dehydration.
Advantages:
 High latent heat of fusion per unit volume.
 Relatively high thermal conductivity.
 Small volume changes on melting
 Inexpensive.
Disadvantages:
 Phase separation.
 Poor nucleation properties.
 Incongruent melting.

b. Metallics:
These are the low melting metals and metal eutectics.

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Advantages:
 High thermal conductivity
 High heat of fusion per unit volume
 Low vapour pressure.

1.3.3 EUTECTICS
Eutectic is a mixture of two or more components with a minimum melting point called
a eutectic point, in which each component melts and freezes congruently forming a
mixture of crystals of components. Eutectics are sub-divided into organic-organic,
inorganic-inorganic and organic-inorganic types.
Advantages:
 Better heat reliability
 Lower phase change temperatures as compared with the corresponding fatty
acids.
 Sharp melting temperature
 High volumetric thermal storage density.

1.4 NEED FOR THE PRESENT STUDY

 Energy consumption in buildings varies significantly during the day and night
according to the demand by business and residential activities
 Phase change materials also have some drawbacks like low thermal conductivity
and liquid leakage during the phase changing process.
 These drawbacks are solved by adding inorganic material as graphite powder into
the fatty acids. Because graphite has some desirable properties like high thermal
conductivity and high thermal stability.

This study focused on the preparation of LA-PA composite as form-stable

PCM by the vaccum absorption method and its characterization by FT-IR
spectrophotometer analysis and determination of its thermal properties . This study
also deals with the improvement of the thermal conductivity of the LA-PA composite
PCM using expanded graphite powder.

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1.5AIM OF THE PROJECT

The aim of the project is to investigate the thermal characterization and

performance of cement mortars incorporated with LA-PA/EG/EP composite phase
change material as thermal energy storage materials.

1.6 OBJECTIVE OF THE PROJECT

 To synthesize the binary fatty acid (Lauric acid & Palmitic acid) based phase
change materials at the desired phase change temperature.

 To determine the thermal characterization by TGA analysis and DSC analysis.

 To improve the thermal stability and thermal conductivity by using Expanded

Graphite Powder.

 To determine compressive strength of the mortar specimens.

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 CHAPTER 2

LITERATURE REVIEW

1. Guruprasad Alva, Xiang Huang, Lingkun Liu, Guiyin Fang(2017) “Synthesis

and characterization of microencapsulated myristic acid–palmitic acid
eutectic mixture as phase change material for thermal energy storage”,
Applied Energy, vol.203, pp.677-685,School of Physics, Nanjing University,
China .

 In this work, microencapsulation is done by using myristic acid -palmitic acid

(MA–PA) eutectic as the core material and silica as the shell material.
 The silica shell material is prepared from Methyl Tri ethoxy Silane and sol gel
technique was used to do microencapsulation.
 DSC was used to measure the thermal properties of the MA-PA/Silica
microcapsules and the results indicated that the melting and solidifying
temperature of the MPCM are 46.08 ℃ and solidifies at 44.35 ℃ with a latent heat
of 169.69 kJ kg-1 and 159.59 kJ kg-1 respectively with minimum supercooling gap
of 1.73℃.
 SEM was used to examine the morphology and particle size of the microcapsules
and it showed that the surface of the shell is smooth and spherical in shape and
having the diameters between 5 µm to 11µm for the microcapsules having PCM to
shell ratio of 1:1.
 The chemical structure of the microcapsules was investigated by using FT–IR and
it is observed that there is no chemical interface between the MA-PA eutectic and
the silica.
 The crystalloid phase of the microcapsules was investigated by using XRD and
there is no variation in crystal structures of both fatty acids and silica shell was
obtained the test results.
 The Thermogravimetric analysis and DTG analysis were used to investigate the
thermal stability of the MA-PA eutectic/Silica microcapsules and the results
showed that the MPCM has good thermal stability.

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2. Yan HE, Xiong Zhang, Yongjuan Zhang, Qin Song, Xiaomin Liao(2016)
“Utilization of lauric acid-myristic acid/expanded graphite phase change
materials to improve thermal properties of cement mortar”, School of
Material Science and Technology, Tongji University, PR China
 Lauric acid-myristic acid/ expanded graphite (LA-MA/EG) composite phase
change materials (PCMs) were prepared by absorbing the binary eutectic mixtures
into expanded graphite(EG) with high absorbability, in which LA-MA binary
eutectic mixture act as latent heat storage materials while EG serves as the
supporting material
 Inner morphology of the prepared LA-MA/EG composite PCMs was observed
through scanning electron microscopy(SEM). Alkali resistance, thermal stability
and thermal properties of the LA-MA/EG composite PCMs were analyzed through
differential scanning calorimeter(DSC), thermogravimetry analysis(TGA).
 Fatty acids also have some drawbacks, such as low thermal conductivity which
obstacles heat transmitting, liquid leakage during the phase change process, the
risk of fume discharge due to the flammable fatty acids.
 These problems are always solved by impregnating fatty acids into porous
inorganic material, for example diatomite, expanded perlite (EP), expanded
graphite(EG) and so on.
 LA-MA/EG composite were prepared by soaking absorption and vacuum
absorption methods. The high porosity and large specific surface area of EG result
in preventing leakage of melted fatty acids.
 LA-MA binary eutectic mixture with molar ratio of 0.66 and 0.34 was proper for
building application, because it has low eutectic temperature of 33.4/°c and latent
heat of 166.8 J/g.
 EG fired at 800°c can absorb as much as 700% LA-MA binary eutectic mixture at
70°c of absorption temperature. The LA-MA/EG composite PCM form stable and
has higher stability as well as thermal conductivity.
 LA-MA/EG PCM based mortar plays a good role in temperature control and delay
the temperature change in model with a decrease of effective heat value.

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3. Hua Zhu, Peng Zhang, Zhaonan Meng, and Ming Li(2015) “Thermal
Characterization of Lauric–Stearic Acid/Expanded Graphite Eutectic
Mixture as Phase Change Materials”,Journal of nanoscience and
nanotechnology,Vol. 15, pp.3288–3294, Solar Energy Research Institute,
Yunnan Normal University, China.

 The eutectic mixture of lauric acid (LA) and stearic acid (SA) is a desirable phase
change material (PCM) due to the constant melting temperature and large latent
heat.

 In the present study, pure LA, SA and the mixtures with various mass fractions of
LA–SA were used as the basic PCMs, and 10 wt% expanded graphite (EG) was
added to enhance the thermal conductivities.
 The LA–SA binary mixture of mixture ratio of 76.3 wt%: 23.7 wt% forms an
eutectic mixture, which melts at 38.99°C and has a latent heat of 159.94 J/g.

 The melted fatty acids are well absorbed by the porous network of EG and they
have a good thermal stability.

 The enhancement of thermal conductivity is due to the reason that EG has multiple
pores and the EG additives form a dense network in the mixture, which increases
the paths of heat conduction.
 EG has a high thermal conductivity of about 4–100 W/mk, hence, the heat is
transferred much more quickly from the outside to the inside via the network
provided by EG.
 In addition, the fatty acids have a good compatibility with EG, which promotes the
heat diffusion in the mixture.
 The microstructures of the mixtures of fatty acids and EG illustrate that the melted
fatty acids can be well absorbed by the multiple pores of EG.
 The measurementsby TPS show that the thermal conductivities of LA–SA binary
mixtures are about 0.32–0.38 W/m. k, and they are increased to about 3.2–3.8
W/m. k by addingEG.

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 Thus the melting temperature, high latent heat and good thermal stability of LA–
SA/EG eutectic mixture make it a great potential for thermal energy storage and
thermal management applications.

4. Antonio Figueiredo, José Lapa, Romeu Vicente, Claudino Cardoso(2016):

“Mechanical and thermal characterization of concrete with incorporation of
microencapsulated PCM for applications in thermally activated slabs”,
Construction and Building Materials, Vol.112, pp.639-647,Department of
Civil Engineering, University of Aveiro, Portugal

 The objective of this study is to quantify the influence of microencapsulated phase

change material (PCM) over the concrete mechanical and thermal properties.
 The PCM incorporation in the concrete was 3.21% by weight of the total mass,
which represents a small percentage of the concrete mixture.
 From the achieved results of the increase of the thermal capacity and a reduction of
the temperature drop is observed for the specimen with PCM.
 The experimental tests on concrete with PCM yielded resistance loss up to 66%
and 52% for compression and bending strength respectively, comparatively with
the reference concrete specimens, without PCM.
 The incorporation of microencapsulated PCM into concrete leads to a reduction in
the concrete mechanical properties with strength losses of 68% in compression,
and 51% in bending were attained.

 From the temperature chamber tests, it was found that the addition of added
quantity of PCM in the concrete slightly improves the thermal behaviour.

 PCM incorporated into the concrete screed layer, can reduce the indoor air
temperature peaks and attenuates the daily temperature swing.

 From the results it is important to conclude that the mixing process and the water
and binder relation must be optimized with higher control levels to reduce the high
strength losses measured.

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5. Sandra Cunha , Marine Lima, Jose B. Aguiar(2016) “Influence of adding
phase change materials on the physical and mechanical properties of cement
mortars”, Construction and Building Materials, Vol. 127, pp. 1–10, University
of Nantes, Saint Nazaire, France.

 The main objective of this work was the study of physical and mechanical
properties of cement mortars with incorporation of non-encapsulated PCM.
 Integration of non-encapsulated PCM did not cause any significant changes in the
water/cement ratio.
 15% decrease in workability was detected in the water content with the
incorporation of 2.5% of phase change material and water/cement ratio.
 There are no changes in density was observed for the integration of non-
encapsulated PCM into the cement mortars.
 Good connection between different materials such as fibres, PCM, binder and
aggregate were observed from SEM.
 Due to adequate mixing and curing of the developed mortars, no cracks were
identified in the microstructure analysis of the non-encapsulated PCM embedded
mortars.
 Reduction of micro porosity of mortars was observed and delayed hardening
process of cement was detected because of the merging of non-encapsulated PCM.
 Pores in mortar were totally or partially occupied by the PCM, so there was a
reduction in the capillary absorption coefficient.
 By immersion also there was a reduction in the water absorption with the
incorporation of PCM which is non-encapsulated.
 It can be concluded from the compressive and flexural strength tests that addition
of non-encapsulated PCM into the cement mortar did not show any changes in the
mechanical behaviour of the cement mortars and also showed high resistance class
which can also be considered into the mechanical behaviour.

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6. Kemal Cellat, Beyza Beyhan, Caner Güngör, Yeliz Konuklu, Okan Karahan,
Cengiz Dündar, Halime Paksoy(2015) “Thermal Enhancement of Concrete by
Adding Bio-Based Fatty Acids as Phase Change Materials”, Energy and
Buildings, Vol.106, pp.156–163¸ Cukurova, University Faculty of Arts and
Sciences, Department of Chemistry, Turkey.

 In this study, binary mixtures of capric acid (CA), myristic acid (MA), lauric acid
(LA), and palmitic acid (PA) were tested as candidate materials for building
applications.

 The melting points of such fatty acid mixtures may further be adjusted, to agree
with human comfort zone temperatures by regulating their compositions.

 Two binary mixtures of CA–LA and CA–MA as candidate PCMs for building
applications.

 The filter paper tests were carried out for three different concrete specimens with
the same PCM contents. We used 10 wt% PCM– much higher than our samples to
be able to detect any possible leakage.

 Results of the tests showed that there was no significant weight change in the filter
papers, before and after heating/cooling cycles.

 Thermal storage capacities were measured to be 109.0–155.4 J/g with a DSC.

 TGA results show that these mixtures can withstand temperatures up to 120°C
without decomposition. This indicates that the PCMs developed here can be used
for passive solar energy storage in buildings.
 Temperature evolution measurements in fresh concrete indicated temperature
increase due to hydration and the setting time could be lowered by adding even
small amounts of PCMs into fresh concretes

 The compressive strengths of 1 wt% PCM added to concrete mixtures were

reduced by 12% yet stayed within the desired limits for C35/45 concretes.

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 When PCM contents were increased to 2 wt%, compression strengths were
reduced further, to be within the limits of C30/37 concretes. Both PCMs were
suitable for self-compacting concrete mixtures used in buildings.

7. Ruilong Wen, Xiaoguang Zhang, Yaoting Huang,et.al (2017) “Preparation

and properties of fatty acid eutectics/expanded perlite and expanded
vermiculite shape-stabilized materials for thermal energy storage in
buildings” Energy and Buildings, vol.139,pp.197-204,School of Materials
Science and Technology, University of Geosciences, China.

 In this study, the fatty acids eutectics (capric acid(CA) and lauric acid(LA)
eutectics) were impregnated into the expanded perlite(EP) and expanded
vermiculate(EVM) to form the two kinds of composite phase change material.
 X-RAY Diffractometer results show that the eutectics with the EP and EVM do not
undergo chemical reaction and only undergo physical combination.
 Thermal conductivity of the CA-LA/EP and CA-LA/EVM was increased
approximately as 89.14% and 87.41% by adding 5 wt% expanded graphite (EG).
 The maximum CA-LA content in EP and EVM was found as 82.93% and 57.48%,
respectively.The thermal cycling test revealed that the composite PCMs had good
thermal reliability and chemical stability even after 200 thermal cycles.
 The FT-IR and XRD results confirm that there is no physical reaction between the
CA-LA and EP, EVM without chemical interaction. The SEM results showed that
CA-LA was successfully retained into the pores of EP and EVM.
 DSC analysis results indicated that the melting temperatures and latent heats of the
prepared CPCMs are in the range of 21–23°C and 81–117 J/g, respectively and
these properties are suitable for thermal energy storage applications in buildings.
 The TGA analysis results signified that the composites have good thermal
durability above their working temperature range.
 Moreover, the thermal conductivity values of the composite PCMs were increased
with EG addition at mass fraction of 5%.

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8. Xiaobin Gu, Peng Liu, Liang Bian, Huichao He(2019) “Enhanced thermal
conductivity of palmitic acid/mullite phase change composite with graphite
powder for thermal energy storage”Renewable Energy,vol.138, pp.833-
841,School of Gemology and Materials Technology, Hebei GEO University,
Shijiazhuang , China

 To improve the energy storage efficiency of phase change composites, porous

mullite was used to encapsulate the PCM-palmitic acid and graphite powder was
applied to enhance the overall thermal conductivity.
 A series of palmitic acid/mullite/graphite (PA/mullite/GP) composites were
prepared to obtain the PA/mullite/GP form stable phase change material (FSPCM)
by facile direct impregnation method.
 Then their microstructure, chemical compatibility and thermophysical properties
were studied by the method of SEM, FTIR, XRD, DSC, TGA and PR,
systematically.
 The DSC results demonstrate that the PA, PA/mullite and PA/mullite/GP have the
enthalpy of melting of 213.1 J/g, 54.7 J/g, and 52.3 J/g, while the enthalpy of
freezing of 217.0 J/g, 53.6 J/g and 51.5 J/g, respectively.
 The thermal conductivity of the prepared PA/mullite/GP has been improved from
0.28W /m. K to 0.52W/m. K owing to the high thermal conductivity of GP.
 The leakage problem of PCM during energy storage process is one of the main
disadvantages of PCM.
 To solve this problem, the porous mullite was used to accommodate PA and then
the PA/mullite composites were fabricated.
 With 5 wt% GP as the addition, the thermal conductivity increased by 86%
compared to the pure PA, which is much higher than other PCMs in literature.
 The addition of GP has greatly improved the overall thermal conductivity of the
fabricated PCM.

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9. Bogdan Diaconu ,Mihai Cruceru, Lucica Anghelescu (2018) “Graphite inserts
for management of thermal conductivity in phase change materials –
performances and limitations” International journal of materials, vol.5,
pp.19-24,Department of Environment and Sustainable Development,
University of Constantin Brancusi, Romania

 The paper presents a discussion on techniques, performances and limitations of

graphite insertion to boost PCMs thermal conductivity.
 The main goals of the paper are to demonstrate that although graphite inserts are
beneficial in increasing the overall efficiency of a PCM – based thermal
management system .
 Graphite insertions in various forms in PCMs offer a significant increase of the
heat conduction, improving to a high degree the thermal performance of the PCM
base thermal system.
 Adding higher concentrations of graphite to the paraffin did not help to reduce the
thermal resistance of the liquid paraffin.
 Graphite has a much higher thermal conductivity than paraffin, but adding a higher
concentration of graphite did not help reduce the thermal resistance.
 This is because of the effect of poor dispersion performance, combination property,
and the solid liquid interface layer.
 The graphite can reduce the temperature difference ratio, but this does not vary
with its concentration. The better combination of the graphite and solid paraffin
can cause lower temperature difference and thermal resistance.
 Four differnet composited with graphite mass fraction 5%, 10%, 15% and 20%
was used.The latent heat of the paraffin-graphite composite decreased from 142.16
J/g (pure paraffin) to 114.90 J/g (paraffin + 20% graphite).
 Nevertheless, the thermal conductivity increased continuously from 0.208 W/(m.K)
(pure paraffin) to 0.874 W/(m.K) (paraffin + 20% graphite).

14
10. Ahmet Sari ,Ali Karaipekli (2009) “Preparation, thermal properties and
thermal reliability of palmitic acid/expanded graphite composite as form-
stable PCM for thermal energy storage” Solar Energy Materials & Solar Cells,
vol.93, pp.571-576, Department of Chemistry, Gaziosmanpasa
University,Turkey

 This study is focused on the preparation and characterization of thermal properties

and thermal reliability of palmitic acid (PA) / expanded graphite (EG) composite
as form-stable phase change material (PCM).
 From differential scanning calorimetry(DSC) analysis, the melting and freezing
temperatures and latent heats of the form-stable PCM were measured as 60.88 and
60.81°C and 148.36and149.66J/g, respectively.
 Thermal conductivities of PA/EG composites including different mass fractions of
EG (5%, 10%, 15% and 20%) were also measured.
 Thermal conductivity of form-stable PA/EG (80/20w/w%) composite (0.60 W/mK)
was found to be 2.5 times higher than that of pure PA (0.17W/mK).
 The PA was confinedin maximum percentageof80wt% without leakage of melted
PCM from porous structure of the EG and therefore, the composite was described
as form-stable PCM.
 The chemical compatibility of PA and EG was characterized using the FT-IR
spectroscopic method. The improvement of the thermal conductivity was also
verified by comparing melting and freezing performance of the PA/EG composite
PCM with that of pure PA.
 Thermal cycling test showed that the form-stable composite pcm had good thermal
reliability and chemical stability although it was subjected to 3000
melting/freezingcycles.
 Based on all results, it was concluded that the form-stable PA/EG (80/20 w/w%)
has considerable energy storage potential for solar LHTES applications because of
its good thermal properties, thermal and chemical reliability and thermal
conductivity.

15
11. Bharadwaj Reddy,C Gunasekar , Atul Shalikrao Mhaske , Mr N
VijayKrishna (2018) “Enhancement of thermal conductivity of PCM using
filler graphite powder materials” IOP Conference Series: Materials Science
and Engineering, vol.402, Department of Mechanical Engineering, SRM
Institute Of Science And Technology.
 The thermal conductivity of paraffin wax which is a phase change materials is
enhanced by adding filler particle Graphite powder to the paraffin matrix. Paraffin
wax is melted in a heating mantle to its melting point of 600ºc.

 Graphite particles are slowly added while the mixture is continuously stirred. SEM
analysis is done to check the interaction between the matrix and the filler particles.
 The graph between thermal conductivity vs volume fraction shows that there is a
rapid increase in thermal conductivity from 80% to 70% paraffin wax
concentration.
 Various results were obtained for the melting time and solidification time of the
composite. The values of thermal conductivity were measured using neilsen’s
equation.
 In SEM analysis, we observe that for 90% paraffin wax, the volume concentration
is very less. But if we observe for 50% paraffin wax, the filler particle
concentration is more.
 There is an increasing trend in the volume concentration when filler particles
concentration is increasing. The slope of the curves in the graphs between melting
point vs volume fraction, solidification time vs volume fraction is almost constant.

 By adding filler particles, the thermal conductivity of paraffin wax is increased.

This results showed that using high thermal conductive fillers are effective for
enhancing the thermal conductivity of PCM.

 In the end we observed that the thermal conductivity value of the paraffin wax is
significantly increased. The highest thermal conductivity is obtained for the
paraffin wax with 70% composition and the value is found to be 2.77w/mk.

16
12. Ahmet Sari ,Ali Karaipekli(2007) “Thermal conductivity and latent heat
thermal energy storage characteristics of paraffin/expanded graphite
composite as phase change material” Applied Thermal Engineering, vol.27,
pp.1271-1277,Department of Chemistry, Gaziosmanpasa University, Turkey.

 This study aimed determination of proper amount of paraffin (n-docosane)

absorbed into expanded graphite (EG) to obtain form stable composite as phase
change material (PCM), examination of the influence of EG addition on the
thermal conductivity using transient hot-wire method and investigation of latent
heat thermal energy storage (LHTES) characteristics of paraffin such as melting
time, melting temperature and latent heat capacity using differential scanning
calorimetry (DSC) technique.
 The paraffin/EG composites with the mass fraction of 2%, 4%, 7%, and 10% EG
were prepared by absorbing liquid paraffin into the EG.

 The composite PCM with mass fraction of 10% EG was considered as form-stable
allowing no leakage of melted paraffin during the solid–liquid phase change due to
capillary and surface tension forces of EG.

 Thermal conductivity of the pure paraffin and the composite PCMs including 2, 4,
7 and 10 wt% EG were measured as 0.22, 0.40, 0.52, 0.68 and 0.82 W/m K,
respectively.

 Increasing the mass fraction of EG from 2% to 10% gradually increased the

thermal conductivity of paraffin/EG composite PCM.
 Melting time test showed that the increasing thermal conductivity of paraffin
noticeably decreased its melting time.

 It was concluded that the composite PCM with the mass fraction of10% EG was
the most promising one for LHTES applications due to its form-stable property,
direct usability without a need of extra storage container, high thermal conductivity,
good melting temperature and satisfying latent heat storage capacity.

17
13. Yan-Hua Bao, Wei Pan, Ting-Wei Wang, Ze Wang et.al (2011)
“Microencapsulation of Fatty Acid as Phase Change Material for Latent Heat
Storage”Journal Of Energy Engineering, vol.137(4), pp. 214-219, ASCE.

 Latent heat storage systems can improve the energy use efficiency and conserve
limited energy resources. Microcapsules of lauric acid (LA) as the core and
melamine formaldehyde (MF) resin as the shell were prepared as phase change
material for latent heat thermal storage by in situ polymerization.
 The obtained microcapsules were characterized in their surface morphology,
particle sizes, thermal properties, thermal cycling, and heat insulation test.
 Scanning electron microscope analysis suggests that the obtained microcapsules
have a spherical shape and smooth surface, and the shell material presents a round
shell layer associated with an inner porous structure.
 Differential scanning calorimeter measurement indicates that the fusion enthalpy of
encapsulated LA is 84.96 J/g, which corresponds to 46.2% by weight of core
content.
 The DSC measurement and accelerated thermal cycling test suggest that
themicroencapsulated LA has good thermal reliability in its stable melting point,
but the fusion enthalpy after 70 thermal cycling has a significant decrease.
 The preceding results showed that the MF/LA microcapsules possess good
potential as a latent heat storage material.
 Packaging PCMs with appropriate melting point on the basis of environmental
requirements by the microencapsulation technique and employing them with
coatings as a kind of new construction material has great possibility in energy
savings and making the indoor temperature adaptable.

14. Lotfi Derradji,Abdelkader Hamid, Belkacem Zeghmatiet al (2014)

“Experimental Study on the Use of MicroencapsulatedPhase Change Material
in Walls and Roofs for Energy Savings” Journal Of Energy Engineering, vol.
141(4),pp.04014046, ASCE.

18
 This paper presents an experimental investigation of a new use of phase change
materials (PCM) as a coating material on concrete and hollow brick walls. Its aim
is to study the influence of the integration of PCM on the thermal behaviour of
cells and on the improvement of thermal comfort in buildings under the Algerian
climate.
 Tests of the flexural strength, compressive strength, bond strength, and hardness
were performed at seven days of age on composite plaster/PCM materials.
 In situ measurements of air and walls temperatures were made in three cells. The
first one was built with traditional materials and the other two with a composite
material plaster/PCM.
 There is an optimum concentration of PCM (30% PCM and 70% plaster) wherein
the composite material has a specific heat and mechanical properties well suited to
the use of this material in the building.
 The measurement results show that the use of a gypsum plaster incorporating 30%
PCM contributes to a reduction of the amplitude of indoor temperature of the cell
by 4°C in the summer. The use of PCM has also improved thermal comfort and
increased the maximum cell temperature by 2°C during winter.
 These results demonstrate that the use of plaster/PCM composites as a coating
provides a real opportunity to achieve energy savings for buildings.

15. Shi Tao, Sun Wei and Yang Yulan(2014) “Characterization of Expanded
Graphite Microstructure and Fabrication of Composite Phase-Change
Material for Energy Storage” Journal of material and civil engineering,
vol.27(4), pp.04014156(1-5), ASCE.

 Phase-change composites for energy storage were prepared by the expanded

graphite (EG) absorption method and their microstructures were analysed.
 The organic phase-change materials (PCMs) were evaluated for their thermal and
latent heat storage properties. The expanded graphite was prepared under the
microwave irradiation.

19
 The scanning electron microscope (SEM) and mercury intrusion porosimetry
analyses showed that expanded graphite had micron-size pores. The EG was able
to easily absorb organic PCMs because of its non-polarity and porosity.
 Composite PCMs for energy storage were fabricated with paraffin and the
expanded graphite. The expanded graphite was blended with paraffin to afford
composite PCM for energy storage.
 The resulting material showed superior heat storage (releasing) effects and reduced
large-range fluctuation in environmental temperature,thus achieving energy
transfer simultaneously across different times and space.

16. Ahmet Sari (2017),” Thermal Energy Storage Properties and Laboratory-
ScaleThermoregulation Performance of Bentonite/Paraffin Composite Phase
Change Material for Energy-Efficient Buildings”journal of material civil
engineering, vol.29(6),pp.04017001-7

 The thermal energy storage (TES) capacity of building materials can be enhanced
by using phase change materials (PCM). In this work, the building composite PCM
was prepared by impregnation of n-heneicosane (HE) as an organic PCM into
bentonite (BNT) clay.
 The chemical, morphological, and thermal characterizations of the developed
BNT/HE composite PCM was performed by scanning electron microscopy (SEM),
Fourier transform infrared (FT-IR), differential scanning calorimetry (DSC), and
thermogravimetry (TG) analysis techniques.
 The SEM and FT-IR results showed that the HE was well incorporated into the
pores of the BNT and had good compatibility with the components of the
composites.
 The DSC analysis results showed that the composite including 36% HE by mass
had a melting temperature of38.32°C and solidification temperature of 38.34°C; in
addition, the composite also can store latent heat of 96.23 J/g and release latent
heat of 94.16 J/g.

20
 The TG analysis demonstrated that the developed composite PCM had good
thermal durability. The thermal cycling test confirmed that the composite had good
long-term thermal reliability and chemical stability.
 The FT-IR results confirmed the presence of good compatibility and weak physical
interactions among the composites components.

2.1SUMMARY OF LITERATURE:

 From the literature, Fatty acids have some drawbacks, such as low thermal
conductivity which obstacles heat transmitting, liquid leakage during the phase
change process.
 These problems are always solved by impregnating fatty acids into porous
inorganic material, for example diatomite, expanded perlite (EP), expanded
graphite s(EG) and so on.
 LA-MA/EG composite can be prepared by vacuum absorption method. The high
porosity and large specific surface area of EG result in preventing leakage of
melted fatty acids.
 LA-MA binary eutectic mixture with molar ratio of 0.66 and 0.34 was found
suitable for building application according to Schroder eutectic equation
 The thermal conductivity values of the composite PCMs can be increased with
addition of EG.
 The graphite can reduce the temperature difference ratio, but this does not vary
with its concentration. A better combination of the graphite and fatty acids can
cause lower temperature difference and thermal resistance.

21
 CHAPTER 3

METHODOLOGY

3.1 GENERAL

The methodology clearly shows the process which have been carried out in this
project. The step by step process of this project is explained in the flow chart. The
process includes the determination of material properties and their application in
mortar .

3.2 METHODOLGY OF THE WORK

The initial process of this project was material collection. The material includes
cement, fine aggregate, bio based fatty acids, graphite etc. The materials were tested to
determine their basic properties and then the samples underwent analytical studies.
Then the specimens were case and tested to find their physical, mechanical and
thermal properties.

22
3.3 FLOWCHART

Problem Identification

Literature Survey

Material Collection and Testing

 FESEM
Material Characterization
 FT - IR

Synthesis of Eutectic Mixture

Thermal Characterization  DSC

 TGA

Casting of Specimens

Mechanical Tests Compressive Strength Test

Thermal Tests

Result and Conclusion

Fig 3.1 Methodology of Work

23
3.4 PROPERTIES OF MATERIALS USED
3.4.1 FATTY ACIDS
Table 3.1 Details of fatty acids
Description Lauric acid Palmitic acid

IUPAC name Dodecanoic acid Hexadecenoic acid

Purity 99% 98%

Molecular formula C12H24O2 C16H32O2

Molecular weight 200.32 256.43

White flakes White crystalline powder,

Appearance
granules or flakes

Odor Slight odor of bay oil Pungent, oily

Density 0.883g/cm3 0.852 g/cm3

Melting point 43-45℃ 61-62.5℃

Boiling Point 225℃ 271.5℃

Solubility Insoluble in water Insoluble in water

3.5 TRIALS CONDUCTED

3.5.1 TRIAL- I: without shell material
 Capric acid and stearic acid taken as the proportion of 0.25:0.75 in a beaker
and they melted and stirred at 300rpm for 30 minutes using magnetic stirrer
equipment to form a eutectic mixture.
 After that graphite powder was added into the eutectic mixture and mixed well
then placed into hot air oven for 4 hours to dry to form a CA-SA/ GP composite.

3.5.2 TRIAL – II: with shell material

24
  Capric acid and stearic acid taken as the proportion of 0.25:0.75 in a beaker
and they melted and stirred at 300rpm for 30 minutes using magnetic stirrer
equipment to form a eutectic mixture.
From the trials conducted, the DSC results obtained was not suitable for the ambient
temperature. So that, the Schroder equation was followed and suitable fatty acids were
taken for calculation of melting temperature for eutectic mixture.
3.6 THEORECTICAL CALCULATION OF MELTING TEMPERAURE FOR
EUTECTIC MIXTURE
∗〲
Melting Temperature −
Where in is the melting temperature of mixture in K,
is the melting temperature of the i-st substance in K,
R is gas constant, 8.315 J/mol.k
is the latent heat of the i-st substance in J/mol

3.6.1 SPECIFICATION OF FATTY ACIDS

Table 3.2 Specification of Fatty Acids

Contents Lauric Palmitic

acid acid

Melting point, °C 42.4 58.9

Latent heat, J/g 286.4 189.6

Molecular weight 200.32 256.42

Gas constant R =8.315 J.mol-1.k-1

Celsius to Kelvin conversion 0o c = 273.15K
J/g to J/mol conversion

1 g of LA = mol of LA
. ā ..

25
 Fig 3.2 Eutectic point graph

On the basis of the calculation formula, the phase diagram can be plotted, and the
eutectic point of the binary eutectic system can be determined. The eutectic point is an
intersection point at which the liquid phase lines A and B intersect. From the graph,
the eutectic point of LA-PA was found as 35.7ºc which is similar to the ambient
temperature .

CHAPTER 4
CHARACTERIZATION TECHNIQUES

26
4.1 DIFFERENTIAL SCANNING CALORIMETER
Determination of the latent heat capacity and melting-freezing temperature in
thermal energy storage materials are very important. With high latent heat, one can
obtain higher efficiency in applications. To determine the thermal properties of phase
change material microcapsules, researchers use differential scanning calorimeter
(DSC). One of the most significant advantages of DSC is the ease and speed with
which it can be used to see thermal changes in microencapsulated phase change
materials. The DSC measures the amount of heat absorbed or released by a sample in
comparison to a standard reference. During measurement; the energy absorbed or
released is recorded as a function of time and temperature. With DSC measurements,
heating and cooling curves of microcapsules are obtained. By analyzing these curves,
the thermal properties and heat storage capacity of microencapsulated phase change
materials can be determined.

Fig 4.1 Differential Scanning Calorimeter

4.2 SCANNING ELECTRON MICROSCOPE

The particle size and the morphological features of microcapsules can be
evaluated using a scanning electronic microscope (SEM). It uses a focused beam of
high-energy electrons to generate a variety of signals at the surface of solid specimens.
Areas ranging from approximately 1 cm to 5 microns in width can be imaged in a
scanning mode using conventional SEM techniques (magnification ranging from 20X
to approximately 30,000X, spatial resolution of 50 to 100 nm).The signals that derive
from electron-sample interactions reveal information about the sample including

27
external morphology (texture), chemical composition, and crystalline structure and
orientation of materials making up the sample.

Fig 4.2Scanning Electron Microscope

4.3 ATOMIC FORCE MICROSCOPY

Atomic force microscopy (AFM) is a type of scanning probe

microscopy (SPM), with demonstrated resolution on the order of fractions of
a nanometer, more than 1000 times better than the optical diffraction limit. The
information is gathered by "feeling" or "touching" the surface with a mechanical
probe. The AFM consists of a cantilever with a sharp tip (probe) at its end that is used
to scan the specimen surface. When the tip is brought into proximity of a sample
surface, forces between the tip and the sample lead to a deflection of the cantilever
according to Hooke's law.

28
 Fig 4.3Atomic Force Microscopy

4.4 FOURIER TRANSFORM INFRARED SPECTROPHOTOMETER

To identify functional groups in organic polymers or compounds and chemical
characterization of MPCMs Fourier transform infrared spectrophotometer (FTIR) was
used. For this purpose, the FTIR spectrum of PCM before and after
microencapsulation was taken. The obtained spectra were compared to determine
whether a change occurred in chemical structures of PCM at the end of the
microencapsulation process.

Fig 4.4 Fourier Transform Infrared Spectrophotometer

29
 IR Spectroscopy by Functional Group
Alkanes
Identification of absorbance 2960-2850 (<3000)
Wavenumbers, cm-1 sp3 C-H stretch
Alkenes
sp2 C-H stretch 3100-3020 cm-1 (>3000)
C=C stretch 1680-1620 cm-1 (often weak)
Alkynes
sp C-H stretch 3333-3267 cm-1
C-C triple bond stretch 2260-2100 cm-1 (often weak)
Nitriles
C-N triple bond stretch 2260-2240 cm-1 (aliphatic)
Alcohols 2240-2222 cm-1 (conjugated)
O-H stretch 3600-3200 cm-1 (strong and broad)
C-O stretch 1150-1050 cm-1

Aromatic Compounds
sp2 C-H stretch 3100-3020 cm-1 (>3000)
C=C stretch ~ 1585 cm-1
Aromatic overtones of ring bends 2000-1667 cm-1
Aromatic out-of-plane ring bends ~ 900-700 cm-1 (see p. 519)
Amines
N-H stretch 3500-3350 cm-1
C-N stretch (often weak and hard to 1250-1020 cm-1 (aliphatic)
find) 1342-1266 cm-1 (aromatic)

4.5 THERMOGRAVIMETRIC ANALYSIS (TGA)

TGA is a method of thermal analysis in which the mass of a sample is
measured over time as the temperature changes. This measurement provides
information about physical phenomena such as phase transitions, absorption and

30
desorption as well as chemical phenomena including chemisorption, thermal
decomposition, and solid-gas reactions (e.g., oxidation or reduction). TGA can be used
to evaluate the thermal stability of a material. In a desired temperature range, if a
species is thermally stable, there will be no observed mass change. Negligible mass
loss corresponds to little or no slope in the TGA trace. TGA also gives the upper use
temperature of a material. Beyond this temperature, the material will begin to degrade.
TGA is mainly used to investigate the thermal stability of polymers. Most polymers
melt or degrade before 200°C. However, there is a class of thermally stable polymers
that are able to withstand temperatures of at least 300°C in air and 500°C in inert gases
without structural changes or strength loss, which can be analyzed by TGA.

Fig 4.5Thermogravimetric Analysis

4.6 COMPRESSIVE STRENGTH TEST
For the determination of compressive strength of various specimens, mortar
sample with dimensions of 70.6 mm length, width and height were used. Specimens
were precured at ambient temperature for 24 hours to remove the moisture content and
after demoulding water curing for 28 days were done for the specimens. And they
were subjected to compression test as per ASTM Standards ASTM C 39-89, with the
rate of loading as 0.15 to 0.34 MPa/sec. The compression strength of the mortar cube
was computed from the fundamental principle,

Compressive Strength =

31
where,
P – Load at failure, N
A – Cross-sectional area, mm2

32
 CHAPTER 5
EXPERIMENTAL INVESTIGATION

5.1 MATERIALS USED

Various materials are used for the production of PCM embedded cement mortar
and tile. The details of these various materials are given below.

5.1.1 Cement

The cement used for this study is Ordinary Portland Cement of 53 grade as per
12269-1987.

Fig 5.1 Ordinary Portland Cement

5.1.1.1 Fineness Test
A 100 g of cement was taken and sieved in a standard IS 90µ continuously for 15
minutes using sieve shaker. The weight of residue left on the sieve is noted.

Table 5.1 Fineness of Cement

S. No Observation Trial 1 Trial 2 Trial 3

1 Weight of cement taken 100g 100g 100g

2 Weight of cement retained 2g 2.2g 2.4g

3 Percentage of residue left on 90µ sieve 2 2.2 2.4

Fineness of cement = (weight retained/weight taken) x 100 = 2.2 %

33
5.1.1.2 Specific Gravity Test

The empty weight of specific gravity bottle is noted as W1 g. The bottle filled
with distilled water and weight taken as W2 g. The specific gravity bottle is filed with
kerosene and weight noted as W3 g. Some of the kerosene is taken out and filled with
cement and the weight is measured as W4 g. Weight of cement is taken as W5 g.

Specific gravity of kerosene = (W3-W1) / (W2-W1)

Specific gravity of cement = [W5 / (W5 + (W3-W4))]

Table 5.2 Specific Gravity of Cement

S. No Observations Trial 1 Trial 2 Trial 3

1 Weight of empty bottle(W1) g 30 30 30

2 Weight of bottle + Water(W2) g 80 80 80

3 Weight of bottle + kerosene(W3) g 70 70 70

4 Weight of bottle + kerosene + cement (W4) g 85 86 85

5 Weight of cement + bottle g 54 53 53

6 Weight of cement(W5) g 20 22 20

7 Specific gravity of cement 3.17 3.14 3.15

Specific gravity of kerosene = 0.8

Specific gravity of cement = 3.15

5.1.2 Fine Aggregate

Aggregates which is passed through 4.75 IS sieve and retained on 75µ

(0.075mm) IS sieve is termed as fine aggregate. Usually, the natural river sand is uses
as fine aggregate. The river sand is screened to remove the inorganic compounds that
are likely to present in it. Ordinary river sand conforming IS 383-1970.

34
 Fig 5.2 Fine Aggregate

5.1.2.1 Sieve Analysis Test

The sample is brought to an air-dry condition before weighing and sieving.

This may be achieved either at drying at room temperature or heating at a temperature
of 1000ºc to 1100ºc. The air-dry sample 1 kg taken and sieved successively on the
appropriate sieves starting with the largest size sieve as started in the table. Sieving is
carried out on a machine not less than 10 minutes required for each test.
Table 5.3 Sieve analysis test for fine aggregate

S. IS Weight % of Cumulative % Cumulative

No sieve retained weight of weight % of Remarks
(mm) (kg) retained retained passing
1 4.75 0 0 0 100

2 2.36 0.015 1.5 1.5 98.50

Sand
3 1.18 0.088 8.8 10.3 89.70
conforming
4 0.60 0.385 38.5 48.8 51.35 to zone II.

5 0.30 0.263 26.3 75.1 24.9

6 0.15 0.199 19.9 95 5.0

7 Pan 0.017 1.7 96.7 3.3

35
 Fineness modulus of sand = Total percentage of cumulative retained/100
Fineness modulus of sand = 3.2

5.1.2.2 Specific Gravity Test

The pycnometer is dried thoroughly and its weight is taken as W1. Fill two third part
of pycnometer with sand and its weighed as W2. The pycnometer is filled with water
up to top without removing sand. Then it is shake well and stirred thoroughly with the
glass rod to remove the entrapped air. After the air has been removed, the pycnometer
is completely filled with water up to the mark. Then outside of the pycnometer is dried
with a clean cloth and is weighed as W3. The pycnometer is cleaned thoroughly. The
pycnometer is completely filled with water up to top. Then outside of the pycnometer
is dried with a clean clothand is weighed as W4.

Table 5.4 Specific gravity for fine aggregate

S. Observation Trial 1 Trial 2 Trial 3

No

1 Weight of empty container (W1g) 460 460 460

2 Weight of container+ sample water (W2g) 750 752 751

3 Weight of container+ sample +water (W3g) 1440 1443 1441

4 Weight of container +water (W4g) 1258 1257 1259

5 Specific gravity 2.665 2.72 2.71

Specific gravity of fine aggregate = (W2-W1)/((W2-W1) –(W3-W4))

Specific gravity of fine aggregate = 2.69

5.1.2.3 Moisture Content Test

Weight of empty china dish is taken as W1. Take some quantity of sand in china clay
dish, and its weight is taken as W2. Place it in oven for 24 hours. After 24 hours, the
sample is again weighed and its weight is taken as W3.

36
 Moisture content of fine aggregate = ((W2-W3) / (W2-W1)) X 100
Table 5.5 Moisture content of fine aggregate

S. No Observation Trial 1 Trial 2 Trial 3

1 Container number 1 2 3

2 Weight of wet soil(W2g) 193 242 228

3 Weight of dry soil(W3g) 183 232 217

4 % of moisture content of fine 5.18 5.31 4.82

aggregate

Moisture content of fine aggregate = 5.1%

5.1.2.4 Water Absorption Test

Take 1000g of fine aggregate (W1). The sample is filled with water and kept for 24
hours. After 24 hours immersion, the sample is taken out and dried in air for getting
the saturated surface dry condition (SSD). Then, it is weighed (W2).

Observations:
W1 of sample taken (W1) = 1000g
W2 of sample in SSD state (W2) = 1010g
Water absorption = ((W2-W1)/W1)) X 100
Water absorption = 1%

5.1.3 Water
A tap water is available in the concrete laboratory is used in manufacturing of the
mortar cubes and tiles. The qualities of water samples are uniform and stable. pH
value lies between 6 and 8. The water is free from organic matter and the solid content
should be within permissible limit as per IS 456-2000 and conforming to IS 3025-
1964.

37
5.1.4 Lauric Acid
Lauric acid also known as Dodecanoic acid occurs naturally in coconut oil. Extra pure
synthesis grade of lauric acid is purchased from Loba Chemie pvt ltd.

Fig 5.3 Lauric acid

5.1.5 Palmitic Acid

Palamitic acid also known as Hexadecanoic Acid, originate from the combined
form of natural animal and vegetable fats. It is the one of the most common long-chain
fatty acids. 98% purity of synthesis grade of palmitic acid is purchased from loba
chemie pvt ltd.

Fig 5.4 Palmitic acid

5.1.6 Expanded Graphite

The high porosity and large specific surface area of Expanded Graphite powder
result in a substantial amount of fatty acids incorporated into the structures, and
prevent leakage of melted fatty acids from the structures.EG present the lowest cost
due to the very limited treatments, and has desirable performances of high thermal
conductivity, high stability, lower weight density, good compatibility with fatty acids

38
from the structures .Due to its slippery nature, graphite and graphite powder valued in
industrial applications for their self-lubricating and dry lubricating properties.

Fig 5.5 Expanded Graphite

5.1.6.1 FESEM ANALYSIS

Fig 5.6 FESEM analysisfor Expanded graphite

39
From the fig 5.6, the yellow arrow shows that crystal form of nature. The expanded
graphite is a crystalline form of the element carbon. The graph shows that the
composition of expanded graphite and it contains higher percentage of carbon about
88.25% , oxygen about 10.97 % and some of silicon and aluminium.

5.1.6.2 AFM TEST Analysis

40
 Fig 5.7AFM results for Expanded Graphite

From Fig 7, the AFM technique is used to elucidate the surface roughness of the
expanded graphite. Fig. (1) represents the 3D topographical image of the expanded
graphite through AFM. Fig (2) is the 2D image of the expanded graphite, from which
the surface characteristics of the material like surface toughness is usually explored
from the line profile analysis drawn through XEI software. Fig (3) on the 2D image, a
horizontal line is drawn at 2.3µm (red line) and from this, it is clear that the surface
having a very small roughness of 17.124nm. A vertical line (green) drawn at the 2D
image at 5.2µm, prove its lower surface roughness of 20.565nm.

5.1.7 Expanded Perlite

Expanded Perlite is an amorphous volcanic glass/ alumina-silicate rock that
hasrelatively high water content, typically formed by the hydration . it has several
properties like low bulk density, high heat resistance, low sound transmission, high
surface area, low thermal conductivity and chemical inertness.

Fig 5.8 Expanded Perlite

41
5.1.7.1FESEM Analysis for Expanded Perlite

Fig 5.9 FESEM images for Expanded Perlite

From the Fig 5.9, the yellow arrow shows no definite shape in the material. The
expanded perlite is a amorphous volcanic glass. The graph shows that the composition
of expanded perlite and it contains higher percentage of oxygen about 48.75% ,
silicon about 34.89 % and some of aluminium, potassium, sodium, calcium, tron,
magnesium and titanium.

42
5.2 MORTAR PREPARATION
Mortar specimens were cast using 1:3 mix and water cement ratio of 0.4.
Cement and Sand were mixed together for 2 minutes and water is added gradually in
required quantity to enhance the workability of the mixes. To this, PCM is added in
two different proportions of 2.5% and 5% by weight of sand and mixed for 2 minutes.
The moulds were cleaned and oil was applied. The mortar mixes prepared in various
proportions was placed in three layers in the mould. For each layer, compaction was
done to fill the voids. At last, finishing is done and excess mortar is removed as shown
in fig 5.11. After 24 hours the specimens were demoulded and subjected to water
curing for 28 days.

5.3 MIX PROPORTION

The mortar and tile specimen are produced by the mixing of sand, cement,
and phase change materials with water in requisite proportions shown in Table 5.6.
Mortar specimen size : 70.6 X 70.6 X 70.6 mm
Tile 1 specimen size : 300 X 300 X 25 mm
Tile 2 specimen size : 230 X 230 X 12 mm

Fig 5.10 Casting of conventional Mortar Specimens

43
 Fig 5.11 Casting of Mortar Specimens

Table 5.6 PCM Mortar Compositions

For one specimen

Composition No of
Specimen Cement Silica Sand MPCM Water
(% ) Samples
(Kg) Fume (Kg) (Kg) (l)
(Kg)
0 PCM 9 0.24 0 0.6386 0 0.088

0 PCM + 9 0.187 0.033 0.6386 0 0.088

15% SF

Mortar 2.5 % PCM 12 0.187 0.033 0.6386 0.0055 0.088

Cube + 15% SF

5 % PCM 12 0.187 0.033 0.6386 0.011 0.088

+15% SF

44
 CHAPTER6
PREPARATION OF LA-PA/EG/EP COMPOSITE

6.1 PREPARATION OF EUTECTIC MIXTURE

 Fatty acid eutectic mixtures were prepared through the melt blending process as
shown in figure.
 The fatty acids (Lauric acid and Palmiic acid) were mixed at varying
proportions of LA: PA as 73.4 :26.6 in a sealed beaker and kept in a water bath
at a constant temperature of 75 - 80℃ until they melt completely.
 The mixture is stirred for 30 min with the aid of the magnetic stirring apparatus
at 300 rpm and then cooled at room temperature.

Fig 6.1 Formation of Eutectic

6.2 PREPARATION OF LA-PA /EG/EP COMPOSITE

Fig 6.2 Procedure for formation of LA-PA/EG/EP composite

45
  Expanded graphite powder was added by 5% and 10% into the prepared
eutectic mixture and its undergoing ultra sonication process to agglomerate the
expanded graphite into the eutectic mixture.
 Then, the expanded perlite was immersed in the final mixture of eutectic and
expanded graphite. This composite was kept in vacuum oven around for 30
minutes to absorb the mixture.
 The expanded perlite mixed composite was kept dry in room temperature after
which coating using sikalatex is done to avoid the leakage of eutectic from the
expanded perlite.
 Sikalatex was prepared by 1:4 ratio with water ,sprayed into the final product of
LA-PA/EG/EP composite.

(a) (b)

Fig 6.3 Formation of LA-PA/EG/EP Composite (a) 5% of EG (b) 10% of EG

46
 CHAPTER 7
RESULTS AND DISCUSSION

7.1 DSC ANALYSIS

(a) (b)

Fig 7.1 DSC Analysis of LA-PA

DSC curve for LA-PA eutectic sample is used to analyse the supercooling
behaviour of the PCM. From the fig 7.1 (a), Melting temperature of the LA – PA
eutectic is 35.25℃ and from fig 7.1 (b), solidifying temperature of the LA – PA
eutectic is 38.01℃. From fig 7.1 (a), the latent heat of melting is 147.708 J/g and
from fig 7.1 (b) latent heat of solidifying is 164.1962 J/g respectively. LA - PA is
having the degree of super cooling of 2.75℃. While comparing the theorectical results
with DSC results, the eutectic point of LA-PA is almost equal. From the above results,
it can be concluded that the MPCM shows good thermal reliability.

7.2FT-IR Analysis

Fig 7.2 represents the FT-IR spectrum of lauric acid, palmitic acid , eutectic
mixture of lauric acid & palmitic acid and LA-PA/5 % of expanded graphite in wave
number unit. From fig 7.2 (a), Peak at 2911.82cm-1 and 2846.44cm-1 are due to the
stretching vibration of the C-H bond in -CH2 and CH3 of the saturate of fatty acids.
From fig 7.2 (a), Peak at 1689.33cm-1 and 1293.39cm-1 are associated with the

47
deformation vibration of the C-H bond in –CH2 group in fatty acids. From fig 7.2 (b)
Peak 699.73cm-1 belongs to the vibration of aromatic out of plane ring bends
compounds of –C-H bending. From fig 7.2 (b), peak at 3564.36cm-1 shows the
vibration of the C-O stretch of carboxylic acids. From fig 7.2 (b), Peak at 3564.36cm-1
and 3449.56cm-1 are due to the vibration of the O-H stretch of fatty acids which is
strong and broad. From fig 7.2 (c), peak at 1692.38 cm-1and 1296.48 cm-1 shows the
bond of the C-C stretch in the eutectic mixture. Peak 2914.61cm-1 in fig 7.2 (c) shows
the sp3 C-H stretch occurred in the eutectic formation. Peak at 1689.30 cm-1 in fig 7.2
(b) shows the vibration of the C-O stretch of aldehydes present in the fatty acids.Thus,
the spectra of the PCM sample retained all the original characteristic transmittance
bands of the fatty acids and expanded graphite. This indicates that there is no chemical
interaction between the fatty acids and the expanded graphite.
(a) (b)

(c)

48
(d)

Fig 7.2 FT-IR Analysis of (a)LA (b)PA (c)LA-PA and (d) LA-PA/5% of EG

7.3 THERMOGRAVIMETRIC ANALYSIS

Fig 7.3 shows the TG/DTA and TG/DTG analysis for LA-PA binary eutectic
with a proportion of 73.4:26.6. From fig (a), the graph indicates there is no weight
loss until 150⁰c. After that, there is a gradual weight loss with respect to temperature
increase. The residual mass value is 1.95 %. The area indicates the latent heat of the
eutectic which is 211.3 J/g. The value shows that it can absorb and store more energy
from the outside.The melting temperature of the LA-MA proportion is about 35.7⁰c
and the weight loss happens due to evaporation only after 150⁰C only. Therefore, it is
negligible. Thus, PCMs have a good thermal stability in their operational range of
temperature.

49
 (a)

Fig 7.3 TGA Analysis (a) TG/DTG/DTA

7.4 COMPRESSIVE STRENGTH OF THE MORTAR SPECIMEN

Cube compressive strength was performed on all the mortar specimens by using
cube compressive testing machine.From the results of compressive strength of the
mortar with varying percentage of PCM as 2.5% and 5%, shows that addition of
PCM into the mortar reduces the strength. For 7 days average compressive strength
with 2.5% of PCM, there is 39.72 % decrease in the strength occurs while adding 5%
of EG and 42.60% reduction occurs with 10% of EG. similarly for 5 % of PCM,
there is 44.28 % reduction while adding 5% of EG and 53.88% reduction occurs
with 10 % of EG. For 7 days average compressive strength with 2.5% of PCM, there
is 22.95 % decrease in the strength occurs while adding 5% of EG and 35.61%
reduction occurs with 10% of EG. similarly for 5 % of PCM, there is 41.34 %
reduction while adding 5% of EG and 41.82 % reduction occurs with 10 % of
EG.Increase in percentage of incorporation of MPCM into the mortar samples lead to
more strength reduction. The strength reduction can be compensated by adding
silicafumes.

50
 Table 7.1 Compressive strength of conventional mortar for 7 and 28 days
7 days 28 days

Load Comp. Avg.comp. Load Comp. Avg.comp.

Specimens kN strength Strength kN strength Strength
MPa MPa MPa MPa

42.2 8.467 91.5 18.470

0 PCM 41.0 8.226 8.366 93.6 18.905 18.530

41.9 8.406 89.5 17.957

0 PCM 53.5 10.734 104.6 20.987

+ 55.7 11.175 10.901 102.9 20.646 20.920
15% SF
53.8 10.794 105.4 21.147

Table 7.2 Compressive strength results of 2.5% PCM for 7 days

7 days

Specimens Load Area Compressive Avg.Comp.

kN Cm2 strength strength
MPa MPa
5% of EG 23.7 49.84 4.755

5% of EG 27.2 49.84 5.457 5.0423

5% of EG 24.5 49.84 4.915

2.5%
PCM
10% of EG 25.0 49.84 5.016

10% of EG 22.6 49.84 5.534 4.8016

10% of EG 24.2 49.84 4.855

51
 Table 7.3 Compressive strength results of 2.5% PCM for 28 days

28 days

Specimens Load Area Compressive Avg.Comp.

kN Cm2 strength strength
MPa MPa
5% of EG 65.6 49.84 13.162

5% of EG 78.8 49.84 15.180 14.276

5% of EG 72.2 49.84 14.486

2.5%
PCM
10% of EG 58.2 49.84 11.677

10% of EG 60.7 49.84 12.178 11.931

10% of EG 59.5 49.84 11.938

Table 7.4 Compressive strength results of 5% PCM for 7 days

7 days

Specimens Load Area Compressive Avg.Comp.

kN Cm2 strength strength
MPa MPa
5% of EG 23.6 49.84 4.735

5% of EG 21.7 49.84 4.353 4.661

5% of EG 24.4 49.84 4.895

5% PCM
10% of EG 17.6 49.84 3.531

10% of EG 20.8 49.84 4.173 3.858

10% of EG 19.3 49.84 3.872

52
 Table 7.5 Compressive strength results of 5% PCM for 28 days

28 days

Specimens Load Area Compressive Avg.Comp.

kN Cm2 strength strength
MPa MPa
5% of EG 54.7 49.84 10.975

5% of EG 54.2 49.84 10.875 10.868

5% of EG 53.6 49.84 10.754

5% PCM
10% of EG 53.7 49.84 10.714

10% of EG 54.9 49.84 11.015 10.780

10% of EG 52.9 49.84 10.613

Fig 7.4 Compressive Strength of 5% of EG Vs Number of Days

53
Fig 7.5 Compressive Strength of 10% of EG Vs Number of Days

54
 CHAPTER 8
CONCLUSION
 Form stable eutectic mixture of lauric acid and palmitic acid with the proportion
of 73.4:26.6 were selected as the main candidate materials to act as the thermal
energy storage materials.
 While incorporating PCM merely into building envelopes, it undergoes leakage
issues. To overcome this problem, expanded graphite and expanded perlite are
preferred and to get the desired operating temperature eutectic LA-PA is used.
 The exothermic and endothermic reactions of the LA-PA were studied by using
DSC analysis. It showed that the melting and freezing temperatures of LA-PA are
35.25℃ and 38.01℃. Then ,the latent heat of melting and solidifying are 147.708
J/g and 164.1962 J/g, respectively.
 From FT-IR analysis, by adding expanded graphite and expanded perlite into the
eutectic mixture, did not cause any chemical interaction between them.
 TGA analysis shows that the weight loss happens after 150oC only. Therefore
PCMs have a good thermal stability at their operational temperature.
 Compressive strength of the PCM mortar specimen decreases with increasing the
percentage of PCM as compared to the control specimen.

55
 CHAPTER 9
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