“Processing, Properties and Thermal Stability of Polymer Derived

Ceramic Foams”
A DISSERTATION SUBMITTED TO THE

VISVESVARAYA TECHNOLOGICAL UNIVERSITY, BELAGAVI

Towards partial fulfillment of the academic requirement for the award of the degree
of
MASTER OF TECHNOLOGY
in
MANUFACTURING SCIENCE AND ENGINEERING
by
KIRAN B
1SI19MSE03
Carried out under the guidance of

Dr. MADHU H C, M.Tech., Ph.D.

Assistant professor,
Dept. of Mechanical Engineering,
S.I.T., Tumakuru

DEPARTMENT OF MECHANICAL ENGINEERING

SIDDAGANGA INSTITUTE OF TECHNOLOGY
(An Autonomous Institute affiliated to Visvesvaraya Technological University, Belagavi,
Approved by AICTE, ISO 9001:2008 Certified)
TUMAKURU – 572 103, KARNATAKA, INDIA
2020 - 2021
 SIDDAGANGA INSTITUTE OF TECHNOLOGY, TUMKUR-572103
(An Autonomous Institute affiliated to Visvesvaraya Technological University, Belagavi, Approved by
AICTE, New Delhi, an ISO 9001:2008 Certified)

DEPARTMENT OF MECHANICAL ENGINEERING

CERTIFICATE
This is to certify that project entitled “Processing, Properties and Thermal Stability of Polymer
Derived Ceramic Foams” is a bonafide work carried out by KIRAN B bearing university seat number
1SI19MSE03 towards the fulfillment of the dissertation work of the academic requirement for the
award of MASTER OF TECHNOLOGY in MANUFACTURING SCIENCE & ENGINEERING
as prescribed by Visvesvaraya Technological University, Belagavi during the year 2020-2021. It is
certified that all the corrections / suggestion indicated during internal assessment have been incorporated
in the report and deposited in the library. The project report has been approved as it satisfies the
academic requirements in the respect of project work prescribed for the above degree.

Project Guide PG Co-ordinator

Dr.H.C.Madhu, M.Tech.,Ph.D. Dr.Virupaxi Auradi, M.Tech., Ph.D.
Assistant Professor, Associate Professor & PG Co-ordinator
Department of M.E., Department of M.E
S.I.T., Tumakuru. S.I.T Tumakuru

Principal
Head of the Department Dr.S.V.DINESH, M.Tech., Ph.D.
Dr.H.R.Purushothama, M.Tech., Ph.D Siddaganga Institute of Technology,
Professor and Head Tumakuru.
Department of M.E.,
S.I.T Tumakuru.

Name of the Evaluators Signature with date

1.

2.
 DECLARATION

I, hereby declare that the project work entitled “Processing, Properties and Thermal Stability of
Polymer Derived Ceramic Foams” has been independently carried out by me under the guidance of
Dr. MADHU H C, Assistant Professor, Department of Mechanical Engineering, Siddaganga Institute
of Technology, Tumkur in the partial fulfillment of the requirements of the degree of MASTER OF
TECHNOLOGY in MANUFACTURING SCIENCE AND ENGINEERING of Visvesvaraya
Technological University, Belagavi during the academic year 2020-2021.

This work has not been submitted in the part or full to any other university for the award of any
degree.

Date: - 16-12-2021 KIRAN B

Place: - Tumakuru (1SI19MSE03)

i
 ACKNOWLEDGEMENT

I submit my reverential pranama’s at the lotus feet of his holiness Dr. Sree Sree Sivakumara
Swamiji and Sree Sree Siddalinga Swamigalu of the Sree Siddaganga Mutt, Tumkur for being a
constant source of inspiration in my life.

I wish to thank Dr. S.V. Dinesh, Principal, Siddaganga Institute of Technology, Tumkur, for
his support and advice.

I wish to thank Dr. Shivakumariah, C.E.O, Siddaganga Institute of Technology, Tumkur, for
his support and advice.

I wish to thank Dr. M.N. Channabasappa, Director, Siddaganga Institute of Technology,

Tumkur, for his support and advice.

I would like to thank Dr. H.R. Purushothama, Professor and Head, Dept. of Mechanical
Engineering, Siddaganga Institute of Technology, Tumkur for his support and advice.

I am also grateful to my project guide Dr. H.C. Madhu, Assistant Professor, Mechanical
Engineering Department, Siddaganga Institute of Technology, for giving me support and
guidance to work my project.

I would like to thank Dr. Virupaxi Auradi, Associate professor & PG Co-ordinator, (MSE),
Dept. of Mechanical Engineering, Siddaganga Institute of Technology, Tumkur for his
support and advice.
I take this opportunity to express my thanks to all the Faculties, staff of the course M.Tech,
(Manufacturing Science and Engineering) Dept. of Mechanical Engineering, Siddaganga
Institute of Technology, Tumkur and my lovable parents for their valuable suggestions.

KIRAN B
(1SI19MSE03)

ii
 Abstract

Ceramic foams have versatile applications as, filters in metal casting process, scaffolds for
catalysts in processing industries etc. Further, they are also being explored for heat shields and
radiation deflectors/absorbers etc. However, traditional methods of synthesizing ceramic foams
i.e. high temperature reaction synthesis, are either not economical or can result in foams with
inferior properties. These issues can be addressed by synthesizing ceramic foams through
polymeric route. In this study, organosilicon Poly Hydrido Methyl Siloxane (PHMS) polymer
was used to synthesize ceramic foams. The PHMS, an organosilicon polymer, was cross-linked
using catalyst to a shape of polyurethane foam used as a scaffold. The cross-linked polymer was
pyrolyzed at various temperatures and durations. Pyrolysis removes organic side chains in the
polymer and results in porous ceramics. Interestingly, the yield of the composite was nearly 70%
irrespective pyrolysis condition. The ceramic foams were characterized using infra-red
spectroscopy, X-Ray Diffraction and Energy Dispersive X-Ray analysis. Microstructural
analysis was done using Scanning Electron Microscopy. The uniaxial compression test was done
to evaluate mechanical properties of these foams. It was seen that compression strength of the
foams increases with pyrolysis temperature and is maximum at 1000°C. Further, the
compression strength also increases with pyrolysis duration, irrespective of the pyrolysis
temperature. The maximum strength of the PDC foam was 5.2 N/mm 2 with excellent toughness
of 200 KJ/m3. Furthermore, it had an excellent thermal stability at elevated temperature i.e.
1000°C up to 5 hours. It can be concluded that PDC route can be excellent cost effective method
to synthesize ceramic foams.
 TABLE OF CONTENTS

Page.No

DECLARATION. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . i

ACKNOWLEDGEMENT . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ii

ABSTRACT . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . iii

LIST OF TABLES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .iv

LIST OF FIGURES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .v

CHAPTER 1 INTRODUCTION

1.1 Introduction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
1.2 Polymers. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .2
1.2.1 Natural Polymers. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
1.2.2 Synthetic Polymers. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
1.3 Organosilicon Polymer. . . . . . . . . . . . . . . . . . . . . . . . . . . 3
1.4 Polymer Derived Ceramics. . . . . . . . . . . . . . . . . . . . . . . . . 4
1.5 Polyhydridomethylsiloxane. . . . . . . . . . . . . . . . . . . . . . . . 5

CHAPTER 2 LITERATURE REVIEW

2.1 Literature Survey . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .6

CHAPTER 3OBJECTS AND METHODOLOGY

3.1 Objects . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
3.2 Process Flow . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 10

CHAPTER 4 MATERIALS AND METHODS

4.1 Materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11
4.2 Synthesis Process . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
4.2.1.1 Preparing PHMS. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
4.2.1.2 Cross-linking Polymer. . . . . . . . . . . . . . . . . . . . . . . . . . . 13
4.2.1.3 Pyrolysis. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
4.3 Microstructural, Compositional and Mechanical Characterization . . . . 14
4.3.1 FTIR. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
4.3.2 SEM and EDX. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
4.3.3 XRD. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
4.3.4 Uniaxial Compression Test. . . . . . . . . . . . . . . . . . . . . . . . .17

CHAPTER 5 RESULTS AND DISCUSSION

5.1 FTIR Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18

5.2 Ceramic Yield . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19
5.3 Microstructural Analysis . . . . . . . . . . . . . . . . . . . . . . . . . 20
5.4 Compositional Analysis . . . . . . . . . . . . . . . . . . . . . . . . . 21
5.5 XRD analysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
5.6 Compression test. . . . . . . . . . . . . . . . . . . . . . . . . . . . . .23
5.7 Toughness of PDC . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
5.8 Thermal Stability. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
5.9 Discussion. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27

CHAPTER 6 CONCLUSION . . . . . . . . . . . . . . . . . . . . . . .29

CHAPTER 7 FUTURE WORK . . . . . . . . . . . . . . . . . . . . . 30

CHAPTER 8 REFERENCES. . . . . . . . . . . . . . . . . . . . . . . 31
 LIST OF TABLES

Table Title Page. No

1 Temperature and Duration used to Pyrolyze Cross-linked Foam . . . . . . . . 13

2 Ceramic Yield of PHMS Foam for Various Pyrolysis Conditions . . . . . . 19

3 Shows ultimate load, maximum deformation and compression strength . . . 25

iv
 LIST OF FIGURES
Fig.No Title Page.No

1 Structure of Organosilicon Polymers. . . . . . . . . . . . . . . . . . . . . . . . .4

2 Processing of Polymer Derived Ceramics. . . . . . . . . . . . . . . . . . . . . 4

3 Molecular formula of PHMS. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5

4 PHMS Polymer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 11

5 Acetone. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12

6 Polymer Pyrolyzed at 600℃ after 3 hours . . . . . . . . . . . . . . . . . . . . 14

7 FTIR testing device Bruker ALPHA II . . . . . . . . . . . . . . . . . . . . . . .15

8 SEM and EDX testing device . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15

9 Rigaku Smartlab X-Ray diffractometer . . . . . . . . . . . . . . . . . . . . . . 16

10 Tinius Olsen 50ST UTM . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17

11 FTIR of (a) Cross linked polymer (b) Polymer pyrolyzed at

600℃ for 3hr and (c) Polymer pyrolyzed at 1000℃ for 3hr. . . . . . 18

12 Density of ceramics vs. Duration of pyrolysis . . . . . . . . . . . . . . . . . 20

13 SEM images of polymer pyrolyzed at (a) 800℃ for 1hr (b) 800℃
for 2hr (c) 800℃ for 3hr (d) 1000℃ for 1hr (e) 1000℃ for 2hr
(f) 1000℃ for 3hr . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21

14 EDX spectrum of polymer pyrolyzed at (a) 800℃ for 3hr and

(b) 1000℃ for 3hr . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22

15 XRD plots of PDCs obtained from various pyrolysis conditions . . . 23

16 Stress-strain curve of polymer pyrolyzed at (a) 800℃ for 1hr

(b) 800℃ for 2hr (c) 800℃ for 3hr (d) 1000℃ for 1hr (e) 1000℃
for 2hr (f) 1000℃ for 3 hr . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24

17 Average compression strength of samples pyrolyzed at 800℃ and

1000℃ . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25

18 Toughness of samples pyrolyzed at 800℃ and 1000℃. . . . . . . . . 26

19 Thermal stability of samples pyrolyzed at 800℃ and 1000℃ for

different durations . . . . . . . . . . . . . . . . … . . . . . . . . . . . . . . . . . . . . 27

20 Compressive strength of β-Ca2 SiO4 scaffolds sintered at different

temperature for 5 hr . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28

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FOAMS

CHAPTER 1

INTRODUCTION

1.1. INTRODUCTION
Ceramics have immensely influenced the development of humanity. Their role in
cutting tools to heat-shields in space applications are noteworthy mentions. Due to
their high hardness, strength and temperature resistance, novel applications for them
are developed every day. Similarly, ceramic foams have a large number of
applications due to their thermo mechanical properties, ease of processing, and
stability at high temperatures. Various methods used to synthesize ceramics are: [1]

1. Powder mixing
Oxides, carbonates and hydroxides are blended and then either wet or dry milled, after
which the powder mixture undergoes repeated calcinations and mechanical grinding
for completion of the solid-state reaction.
2. Fusion
In the fusion route, oxides and carbonates are melted together and after solidification,
lumps are ground into ceramic powders by mechanical grinding.
3. Sol-Gel Processing
The sol-gel method is a method, for material preparation under mild conditions,
involves ceramic synthesis by hydrolysis of metal-organic compounds.
4. Gas-Phase Reactions
Reactions between gases, or between solids and gases, are used for the synthesis of
ceramics, particularly non-oxides.
5. Hydrothermal Synthesis
Mono dispersed ceramic powders can be obtained by heating salt solutions under
hydrothermal conditions.
6. Non-aqueous Liquid-Phase Reactions
Liquid-phase reactions take place in a non-aqueous solvent, which may be inert or one
of the reactants, and are associated with the synthesis of non-oxide powders,
particularly Si3N4.
7. Polymer derive ceramic route
Polymer pyrolysis is also known as Polymer-Derived Ceramic technique which
refers to the synthesis of a polymeric compound, sometimes called a preceramic
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polymer, which is then fabricated into a certain shape and pyrolyzed to the ceramic
in an inert atmosphere.
Polymer derived route trumps over other methods because

 Reduced processing temperature

 High strength in the green state
 Flexibility in shaping the ceramic
 Improved ceramic yield

1.2. POLYMERS
Polymers are materials consisting of long-chain repeating units of molecules. These
materials have properties depending on molecules present in the polymer chain.

Polymers are of two types

1) Natural polymers
2) Synthetic polymers
1.2.1. Natural polymers
Natural polymers contain simple hydrocarbon in their chain. Proteins, wood,
and rubber are examples of natural polymers
1.2.2. Synthetic polymers
Man-made polymers are termed synthetic polymers.
They are broadly classified
I. Based on deformation
i) Thermosetting polymers: the polymer which is deformed on heating
cannot be reversed again on applying heat. Example Bakelite, Epoxy
Resins.
ii) Thermoplastic polymers: the polymers which are deformed on heating can
be reversed again on applying heat. Example: polyethene, polypropylene.
II. Based on molecules present in the chain
i) Organic polymers: polymers that contain carbon as the backbone in the
polymer chain. Example polystyrene, polyvinyl chloride.
ii) Inorganic polymers: polymers that do not contain carbon atoms in the
chain. Example: polysilanes, polysiloxanes.

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iii) Hybrid polymers: polymer containing both organic and inorganic

components in the chain. Example: poly(dimethylsiloxane),
Polymethylhydrosiloxane.
Inorganic and hybrid polymers when pyrolyzed at suitable temperatures lose their side
chains and result in ceramics.

1.3. ORGANOSILICON POLYMER

These are the hybrid polymers containing carbon and silicon bonds as repeating units.
This is mainly used to produce silicon-based ceramics. By adjusting the organosilicon
polymer, the properties of ceramics can be controlled. To achieve this polymer should
possess high molecular weight, suitable viscoelasticity properties, shaping properties
and curing properties i.e. thermosetting.
Types of organosilicon polymers

i. Polysilane
ii. Polycarbosilane
iii. Polysilazane
iv. Polysiloxane
v. Other organosilicon polymers

1.3.1 Polysilane: It is an organosilicon polymer with a simple 1-Dimensional silicon

backbone. Example: Poly(dimethylsiloxane)

1.3.2 Polycarbosilane: its structure is complex due to the presence of different forms
of carbon chain in the backbone like methylene, phenylene etc. Example:
Polydimethyl-methylsilane

1.3.3 Polysilazane: Organosilicon polymer containing alternating silicon-nitrogen

bond with carbon side groups in its backbone. Example: Hexamethyldisilazane

1.3.4 Polysiloxane: Organosilicon polymer containing silicon-oxygen backbone with

some organic groups. Example: Polymethylhydrosiloxane.

1.3.5 Other organosilicon polymers: polycarbosilane, polyborosilazane,

polyborosilocone are other organosilicon polymers.

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Figure 1: Structure of Organosilicon Polymers [2]

1.4. POLYMER DERIVED CERAMICS (PDC’S) ROUTE

Figure 2: Processing of Polymer Derived Ceramics [2]

In the PDC’s route, organosilicon polymer is chosen as the preceramic material which
is subjected to heating in a controlled atmosphere results in ceramics with desired
properties. The microstructure of these ceramics can be tuned by proper controlling
organosilicon polymer chemistry and the processing parameters to tailor-make
products suiting to the specific requirements of a particular application. Polymer-
derived ceramics technique shows plenty of advantages for the fabrication of
advanced ceramics. Processing of organosilicon polymers involves the synthesis of
organosilicon polymers, shaping, cross-linking, pyrolysis, and ceramization and
subsequent processes to synthesize silicon-based ceramics.

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1.5. POLYHYDRIDOMETHYLSILOXANE (PHMS)

Figure 3: Molecular formula of PHMS [4]

Polyhydridomethylsiloxane is a linear polymer containing silicon–oxygen-silicon

backbone with one methyl group attached to silicon and one hydrogen attached to
silicon. This is formed by hydrolyzing methyldichlorosilane. PHMS is the by-product
of the silicone industry. It is cheap, easy to handle and environmentally friendly and it
can be produced directly or by ring-opening polymerization of the cyplyomers. PHMS
is a very low viscosity liquid and has a density close to water. It is moisture stable and
can be stored for long periods without loss of activity. [4]
Polymer derived ceramic route (PDC) is advantageous because the structure of the
ceramics can be tuned by controlling organosilicon polymer chemistry. Tailor-make
products suitable for specific requirements can be produced. As the processing
temperatures reduce, high in the green strength, and improved ceramic yield than
other methods.

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CHAPTER 2

LITERATURE REVIEW

2.1 LITERATURE SURVEY

In the literature survey, different techniques for the manufacturing of ceramics are
explained by Akshay Kumar in which covers the traditional method of powder mixing
to the modern method of polymer derived ceramics. It also covers various aspects of
advanced ceramics like carbides, nitrides and oxides for environmental application.
This book focused on nanostructured ceramics synthesis, properties of their
application to environment. [1]

Polymer derived ceramic (PDC) route to synthesize ceramics is explained by

shengyang et al in a review paper summarizing the different types of organosilicon
polymers, processing of these organosilicon polymers. Also to synthesize silicon
based ceramics from these polymers using the PDC route. This paper mainly
highlights the three-dimensional (3D) printing technique for shaping the organosilicon
polymer. It helps the possibility of fabricating silicon-based ceramics with complex
structures. [2]

Paolo Colombo et al have reviewed PDC technology from its origin. In this article the
general processing techniques to produce different types of Si based preceramic
polymers like silicon oxycarbide and silicon carbonitride based ceramics were
highlighted. Micro structural features of PDCs of SiCO and SiCN which depends on
type of preceramic material, carbon content, and temperature of pyrolysis process and
atmosphere of pyrolysis are explained. Properties of PDCs that are related to their
unique nanosized microstructure are included. [3]

Various organosilicon polymers available for synthesizing Ceramics by PDC route

were illustrated by Jessica D. Torrey et al. In this paper six organosilicon polymers
like poly(silsesquioxane) polymers and polysiloxane polymers were considered for
the study. Metal powders and intermetallic materials like Al, Cr, Fe, Si, Ti and TiSi 2
were taken as potential expansion agents. In this study, the most desirable polymer
and expansion agent combination and their optimal processing parameters have been
highlighted. Ceramic yield percent in various atmospheres like air, nitrogen and
helium are reported. [4]
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PHMS was used to synthesize ceramics by Y.D.Blum in his thesis. This thesis deals
with the availability, synthesis and modification of PHMS. Blum explains the
development of preceramic polymers for various coating applications. It also explains
Si-based polymers can be tailored to be precursors. PHMS can be modified by
dehydrocoupling reactions catalyzed by Pt and Ru. It explains the organic and
inorganic modifications of PHMS for coating applications. [5]

The different methods to produce foams in ceramics was explained by cekdar et al,
explaining different processing strategies to obtain ceramic foams, such as replica
method, sacrificial template method, direct foaming technique, etching, aerogel
foaming method, fiber spinning and automated manufacturing methods. Pore size,
porosity and strength of ceramics obtained by all these methods are highlighted. [6]

Colombo et al reported on controlling porosity in ceramics. They have reported that

porosity in ceramics produced by the PDC route can be increased to more than 70%.
They have also reported novel methods to synthesize porous ceramics by direct
foaming and sacrificial fillers. In this report they have opted for controlled
atmosphere heat treatment, the addition of with large surface area to the polymer. By
this method, ceramic foams of various shapes can be produced. [7]

Further, Colombo et al have reported the synthesis of SiOC ceramics by direct

foaming method, includes pyrolysing preceramic polymer with polyurethane solutions
and Preceramic polymer with blowing agent solutions. A comparison of mechanical
and elastic properties is made between this method and commercial foams produced
by a conventional method. The ceramic foam produced by this method and pyrolysing
in an inert atmosphere can develop good strength in ceramics, near net shape can be
produced, lightweight and ceramic foam with good high temperature resistance can be
produced. [8]

Articles by Ju¨rgen Zeschky et al shows the one step manufacturing process to

produce Silicon Oxycarbide foams where Si and SiC loaded to polymer
methylphenylpoly(silsesquioxane). This mixture was blended using a ball mill. This
blend was heat-treated and then pyrolysed in nitrogen. Further, a porosity gradient can
be generated by varying the foaming temperature. This paper highlights the relation
between the surface area to volume ratio, the connectivity density and the mean strut
thickness and processing temperature. [9]
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Lixia Wang et al have shown SiOC ceramics derived from siloxane polymers with
different side groups can influence of carbon content electrical conductivity, thermal
stability and phase evolution. This article highlights the relation between carbon
content, ceramic yield, and bulk density. The SiOC samples show high thermal
stability in the air up to 690–860 °C. The highest electrical conductivity is 705.3 S
m−1 at 403 °C. [10]

Ralf et al report the synthesis, characterization, processing of organosilicon polymer

derived ceramics materials. The ceramics were prepared by heat-treating of
precursors. This paper highlights the effect of polymer molecular structure on the
properties of ceramic materials obtained. It also explains the practical applications of
polymer-derived Si-based ceramics. In the PDCs route, commonly used organosilicon
polymers are polyorganosilylcarbodimides, polyorganosilazanes and
polyorganosiloxanes. In this, materials can be easily shaped to any size or shapes. The
PDCs shows very good thermo mechanical properties. In this paper the compositional
and micro structural analysis is done on PDC. It is observed that the change in
macroscopic properties is because of the variation of composition and solid-state
structure of these materials. [11]

Mechanical properties of ceramics obtained by PDC route are highlighted by

I.M.Daniel et al. In this report, silicon carbide with varying densities were
investigated. The cupons were tested under pure shear and uniaxial compression test.
Stress-strain curve were drawn for the above tests. Shear strength and ultimate shear
strain were determined. Weibull distribution function was used to determine
differences in the result obtained by different test methods, specifically for three-rail
shear and torsion test results. It highlights that the Young’s modulus changes linearly
with relative density of foam. [12]

From the above literature, it can be stated PDC technique can be used to synthesize
ceramics. From the literature, it can be seen that ceramic foams synthesized through
PDC route are promising for high-temperature application. However, studies on their
stability at those temperatures are sparse.

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CHAPTER 3

OBJECTIVES AND METHODOLOGY

3.1 OBJECTIVES

1. To synthesize polymer derived ceramics foams from organosilicon precursor

polymer using the PDC route.
2. To analyze microstructure and composition of ceramic foams.
3. To evaluate the effect of pyrolyzing temperature and time on ceramic yield.
4. To evaluate the effect of pyrolyzing temperature and time compressive strength,
the toughness of ceramics foams.
5. To evaluate high-temperature stability of synthesized ceramic foams

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3.2 PROCESS FLOW

The methodology followed in this present work is in the below flow chart.

PHMS Catalyst

Impregnating PMHS on
Polyurethane foam scaffold

Resting the impregnated PU

foam for 8hrs for cross-linking

Pyrolyzing cross-linked foam

at various duration and time

Characterization of Foam

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CHAPTER 4

MATERIALS AND METHODS

The materials used for synthesis, processing and characterization methods are
illustrated in this chapter

4.1 MATERIALS
The materials used to synthesize the ceramic foams are as follows:
1. Polymethylhydrosiloxane (PHMS)
2. DABCO (1,4[diazabicyclo2.2.2] octane)
3. Acetone
4. Polyurethane foam

4.1.1 Polymer PHMS

Polyhydridomethylsiloxane is a linear polymer containing silicon–oxygen-silicon
backbone with one methyl group attached to silicon and one hydrogen attached to
silicon. This is formed by hydrolyzing methyldichlorosilane. PMHS was selected to
synthesize ceramics because of its aviliability, non-toxicity and cost effectiveness.

Figure 4: PHMS Polymer

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4.1.2 DABCO
The PMHS polymer needs to be cross-linked before pyrolysis to obtain a near-net
shape. The cross-linking can be done either by heating or use of catalyst. In the
current case, PHMS is cross-linked using DABCO, a bicyclic organic compound. The
molecular formula of the DABCO is given by N 2(C2H4)3. It is used as base catalyst
and a reagent in polymerization and organic synthesis. Further, the cross-linking time
can be varied by varying percentage of DACO. [13]

4.1.3 ACETONE
Acetone which also known as propanone, it is an organic compound with molecular
formula (CH3)2CO, It is a colorless highly flammable liquid with high volatility and
pungent smell. The acetone is used to dissolve catalyst DABCO and blended with
PMHS for cross-linking.

Figure 5: Acetone

4.1.4 Polyurethane foam

Polyurethane foam is a porous synthetic material made from the reaction of polyols
and diisocyanates. It has good thermal insulation, high absorption, low density and
high flexibility. It is used in mattresses, car seats and for packing materials. In this
work, it is used as a scaffold to synthesize foam of the required shape and size. PU
foam having a density greater than 44Kg/m3 are termed as high-density foams. In this
study PU foam with a density between 60 and 65Kg/m3 and pore size ranging from 50
to 1000µm is used.
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4.2. Synthesis process of polymer derived ceramics foams (PDCs)

4.2.1. Steps to synthesis PDC:
1. Preparing PHMS for cross linking
2. Cross linking polymer
3. Pyrolysis

4.2.1.1 Preparing PHMS:

PHMS is degassed to remove volatile liquids hence reduce shrinkage and cracks in
pyrolyzed ceramic. Degassing is by heating polymer in a furnace between 100℃ to
120℃.

4.2.1.2. Cross-linking of polymer

Cross-linking is process by which the individual polymer chains are linked. The
cross-linking is carried out to provide shape the polymer, increase its stability and to
reduce water retention. In this study cross-linking is done by blending PMHS with
DABCO solution (5% by weight) and impregnating PU foams. The impregnated foam
is undisturbed for eight hours to complete cross-linking reactions. After cross-linking
polymeric foam is pyrolyzed to obtain ceramic foams.

4.2.1.3. Pyrolysis
After cross-linking for eight hours impregnated in liquid was solidified. This
solidified foam was pyrolyzed. The cross-linked foam was pyrolyzed at temperature
and durations as show in the Table 1. During pyrolysis the organic compounds present
in the polymer chain are eliminated and Si-O and Si-C bonds remain.

Table 1: Temperature and duration used to pyrolyze cross-linked foam.

Temperature Time (hours)

(℃)
600 1 2 3

800 1 2 3

1000 1 2 3

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Figure 6: Polymer Pyrolyzed at 600℃ after 3 hours

It was observed that all samples pyrolyzed at 600℃ were appeared to be partially
converted, as seen in Figure 6. The samples showed sporadic dark light areas
distributed over the bulk of the samples. The appearance of samples pyrolyzed at
800℃ and 1000℃ was more uniform and seems to withhold porous structure of the
foam. Hence, for further studies only sample pyrolyzed at 800℃ and 1000℃ were
considered.

4.3. Microstructural, compositional and Mechanical Characterization

The following test are conducted on the pyrolyzed samples
1. Fourier Transform Infrared test (FTIR).
2. Scanning Electron Microscopy test (SEM) and Energy Dispersive X-ray
Analysis (EDX).
3. X-Ray Powder Diffraction (XRD)
4. Uniaxial compression test

4.3.1 Fourier Transform Infrared test (FTIR)

FTIR is a nondestructive technique that can be used to obtain infrared spectrum of
absorption or emission of solid, liquid or gas. The spectrometer collects high
resolution spectral data over a wide spectral range of frequencies. The FTIR device
used in this study is Bruker ALPHA II.

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Figure 7: FTIR testing device Bruker ALPHA II

The device contains Attenuated Total Reflection (ATR) to enhance the surface
sensitivity, Diffuse Reflectance Infrared Fourier Transform Spectroscopy (DRIFT) it
operates by directing the infrared radiation (IR) into a sample cup and External
Reflection Modules. FTIR analysis is done by measuring the infrared region that are
absorbed by a material. This is achieved by the application of IR to samples. Different
material absorbs IR in various wavelengths. This IR is absorbed by the material at
different wavelengths is measured to determine the composition and structure of
material. Materials are identified by searching the spectrum against a database of
reference spectra. The sample thickness ranges from 0.1 to 10 µm.
Testing Process: Placing sample in FTIR spectrometer, this spectrometer directs the
beam of IR at the samples. It measures how much and at which frequency the samples
absorb the IR

4.3.2 Scanning Electron Microscopy test (SEM) and Energy Dispersive X-ray
Analysis (EDX).

Figure 8: SEM and EDX testing device

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SEM is used to analyze structure of the foams produced. For this SEM, JEOL JCM
6000 PLUS was used. JEOL JCM 6000 PLUS can magnify up to 60,000X, with a
resolution of 10nm. It works on the principle of applying kinetic energy to produce
signals on the interaction with electrons. These electrons are secondary electrons,
backscattered electrons and diffracted backscattered electrons which are used to view
crystallized elements and photons. The secondary and backscattered electrons are
used to produce an image. The secondary electrons emitted from the specimen play
the primary role of detecting the morphology and topography of the specimen while
the backscattered electrons show contrast in the composition of the elements of the
specimen.EDX was used for compositional characterization. It works on the
measuring energy of X-rays released during interation of accelerating electrons.

4.3.3 X-Ray Powder Diffraction (XRD)

It is a technique used to determine the crystallographic structure of material. It works
by exposing a material with X-Rays and measuring the intensity and scattering angles
of x-ray reflected from the material. It can also be used to determine material
composition by the diffraction pattern, phase identification, strain, grain size, atomic
arrangements, phase composition etc. It works on the principle of Bragg’s Law i.e.
when the x-ray is incident onto a crystal surface, its angle of incidence, will reflect
with the same angle of scattering and the path difference is equal to a whole number
of wavelength constructive interference will occur. For XRD analysis Rigaku
Smartlab X-Ray diffractometer was used. The XRD is carried out on pyrolysed
samples i.e. 600℃ 1hr and 3hr,800℃ 3hr, 1000℃ 1hr and 3hr.

Figure 9: Rigaku Smartlab X-Ray diffractometer

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4.3.4 Compression Test

It is one of the fundamental mechanical tests used to determine mechanical behavior
of materials. The compression test was done as per ASTM C1424 standards; this
standard is used to determine the compressive strength of advanced ceramics at
ambient temperature. The compression test was performed by placing a sample in a
Universal Testing Machine (UTM) with the fixtures and load is applied and until
failure. Tinius Olsen 50ST Universal Testing Machine (UTM) with capacity up to
50kN was sued to conduce compression Tests. The compression test was carried out
in ambient condition. The cubes of length 10mm were used as compression samples.

Figure 10: Tinius Olsen 50ST UTM

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CHAPTER 5

RESULTS AND DISCUSSION

5.1 FTIR of cross-linked and pyrolyzed foam specimen

The cross-linked polymer and pyrolyzed ceramic was subjected to FTIR analysis to
identify the chemical bonds present in the samples. The graphs are plotted on data
obtained on sample’s absorbance of infrared light and various wavelengths.

Figure 11: FTIR of (a) Cross linked polymer (b) Polymer pyrolyzed at 600℃ for
3hr and (c) Polymer pyrolyzed at 1000℃ for 3hr

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The FTIR graph showed in Figure 11(a) shows cross-linked PHMS, with peaks
corresponding to Si-C, Si-H, and C-H bonds. The graph in Figure 11(b) and 11(c) of
polymer pyrolyzed at 600℃ and 1000℃ for 3hr respectively did not have any peaks
indicating that all bonds were broken and the organic side chains were eliminated.

5.2 CERAMIC YIELD

Amount of ceramic obtained from the polymer is critical parameter that will
determine the viability of the precursor. Hence, ceramic yield was calculated as a
percentage of initial polymer weight and is listed in Table 2.
Table 2: Ceramic yield of PHMS foam for various pyrolysis conditions

Temperature (℃) Time (hour) Ceramic yield (%)

1 70.4±1.68

800 2 69.2±4.50

3 72±0.78

1 73.6±4.76

1000 2 72.6±3.74

3 65.4±8.54

As it can be seen the irrespective of the pyrolysis condition, the ceramic yield the
samples are about 70%. The pyrolysis conditions that have lower ceramic yield have
a larger standard deviation. Hence, the variations in yield can be attributed
variability of structure of the polyurethane foam scaffold. This is due to variation in
scaffold wall thickness and pore distribution. The yield of polymer is a function of
molecular weight, degree cross-linking and oxidation of polymer during pyrolysis. In
the current case, as molecular weight of polymer and cross-linking is identical for
polymer, they are less likely to cause variation in yield. The oxidation of polymer
mainly depends on the exposed surface area. The variation in scaffold structure
results in the variation of exposed surface area, hence leading to variation in ceramic
yield. Further graph shows that density of samples increases with increase in

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pyrolysis temperature and time is given in Figure 12.

Figure 12: Density of ceramics vs. Duration of pyrolysis

5.3 MICROSTRUCTURAL ANALYSIS

SEM analysis was carried out to analyze surface morphology of the pyrolyzed
samples. As it can be seen from the figure 13, pore structure is well defined and
replicates the structure of the PU foam. The pore sizes were nearly identical for all
samples pyrolyzed at different conditions. Pyrolyzed samples did not show micro
cracks and had considerable wall thickness. However, sample pyrolyzed at 1000ºC
for three hours had large and micro cracks distributed in its structure.

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Figure 13: SEM images of polymer pyrolyzed at (a) 800℃ for 1hr (b) 800℃ for
2hr (c) 800℃ for 3hr (d) 1000℃ for 1hr (e) 1000℃ for 2hr (f) 1000℃ for 3hr

5.4 COMPOSITIONAL ANALYSIS

To know the composition of pyrolyzed samples EDX analysis was done. Molecular
formula of PHMS shown in Figure 3 shows the presence of large number of C-H
bonds. But EDX spectrum of pyrolyzed samples shown in Figure 14 indicates C-H
bond is broken.
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Figure 14: EDX spectrum of polymer pyrolyzed at (a) 800℃ for 3hr and
(b) 1000℃ for 3hr

5.5 XRD RESULT

To analyze the phases formed from pyrolysis XRD analysis was carried out on
cross-linked PHMS and samples pyrolyzed at different temperatures (figure 15). The
cross-linked PHMS showed a broad peak at 15º. The sample pyrolyzed at 600℃ for
one hr showed a similar peak that was shifted by 5º, indicating that the initial
composition was still not altered. As the pyrolysis duration increases to three hrs,
these peaks had broadened indicating a change in the initial phases. However, it was
seen that the pyrolysis was complete (Figure 15). All other curves were nearly
identical, with a broad initial peak. The absence of sharp peaks is characteristic of
PDC’s synthesized below 1000℃, due to the nano crystalline amorphous structure
of ceramic obtained. Further, the sample pyrolyzed at 1000℃ for three hours shows
a sharp peak corresponding to carbon resulting from pyrolysis.

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Figure 15: XRD plots of PDCs obtained from various pyrolysis conditions

5.6 COMPRESSION RESULTS

The compression test was carried out and the stress-strain curved are plotted in
Figure 16. Typical to foam structures, compression curves of PDCs show
considerable variability in maximum stress and strain of samples pyrolyzed at same
conditions. Further, the curves show a jagged profile corresponding to fracture of
cell walls with increasing load. The compression strength and maximum strain till
fracture are shown in Table 3. There is a marked increase in the maximum stress of
samples pyrolyzed at 1000℃ as compared to 800℃ samples. Further, it was seen
that maximum stress peaks at two hours of pyrolysis. Figure 17 shows the average
compression strength vs. temperature, which indicates an increase in compression
strength over an increase in pyrolysis temperature.

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Figure 16: Stress-strain curve of polymer pyrolyzed at (a) 800℃ for 1hr (b)
800℃ for 2hr (c) 800℃ for 3hr (d) 1000℃ for 1hr (e) 1000℃ for 2hr (f) 1000℃
for 3 hr

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Table 3: Shows ultimate load, maximum deformation and compression strength

Temperature Time Ultimate Load Maximum Average

(℃) (hour) (N) deformation Compression
(mm) strength
(N/mm2)

1 155.2±25.76 0.15±0.031 1.1±0.17

800 2 201.3±21.94 0.15±0.072 1.5±0.25

3 242.8±59.4 0.14±0.012 1.4±0.32

1 235±18.2 0.13±0.024 1.6±0.04

1000 2 303.8±137.8 0.14±0.012 3.2±1.22

3 520.9±168.2 0.15±0.078 2.8±1.72

Figure 17: Average compression strength of samples pyrolyzed at 800℃ and

1000℃

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5.7 TOUGHNESS OF PDC

Toughness is defined as the ability of the material to absorb energy until fracture
when subjected to loading. It can be evaluated by the area under the stress-strain
curve of the material subjected to uniaxial loading. The toughness of PDCs is
calculated from compression test. (Figure 18). From the graph, it can be seen that the
samples pyrolyzed at 1000℃ have higher toughness than 800℃ samples. Further, it
can also be seen that the toughness of 800℃ samples monotonically increases with
pyrolysis duration, whereas 1000℃ peaks at two hours. It was observed from SEM
(Figure 13) micrographs that in 1000℃ three hour pyrolyzed sample, large number of
microcracks were present which under loading consolidated reducing the toughness of
the composite.

Figure 18: Toughness of samples pyrolyzed at 800℃ and 1000℃

5.8 THERMAL STABILITY

The pyrolyzed samples were heat-treated to 1000℃ up to 5hrs to study their stability
under elevated temperature in oxidizing atmosphere. It can be seen from except for
the initial drop in the weight the ceramic foam is stable throughout the duration of the
testing i.e. 5 hrs. The initial weight loss of all samples is within10%. Further it is also
interesting to note that even the samples pyrolyzed at 800℃ had stability similar to
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samples pyrolyzed at 1000℃. This indicates polymer to ceramic conversion is

complete even at 800℃. One of the major issues of silicon-based ceramics ready
oxidation in elevated temperatures, which is expected to increase with porous
structure, has been addressed.

Figure 19: Thermal stability of samples pyrolyzed at 800℃ and 1000℃ for
different durations.

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5.9 DISCUSSION
Ceramic yield of PDC was found to be 70% because of the removal of organic
elements present in polymer PHMS during pyrolysis. During pyrolysis stage the
hydrogen bond with carbon will be broken and it is released in the form of gas.
Polymer PHMS which is a waste of silicon industry which is cheap and easily
available is used to produce PDC. PDC are pyrolzed from 600℃ to study their
properties but it was found that conversion from polymer to ceramic is incomplete at
600℃ as shown in figure 6. The sample which is pyrolysed at 600℃ shows sporadic
dark light areas distributed over the bulk of the sample represent it is not pyrolyzed
completely, this is because the energy required to break the bond between hydrogen
and carbon is not sufficient at 600℃, hence samples pyrolyzed at 800℃ and 1000℃
were characterized further.

Figure 20: Compressive strength of β-Ca2 SiO4 scaffolds sintered at different

temperature for 5 hr. [2]

Figure 20 shows compression strength of PDC prepared by 3D printed pores, with

fillers CaCO3 and with temperature higher than 1000℃ for duration 5hr. The PDCs
synthesized at 1000℃ in current work shows the compression strength relatively
higher than this without fillers as well as lower pyrolysis temperature and durations.
From this study,
 Compositional and microstructural analysis: Properties are used to examine
that PDC route can be used to synthesize ceramics.
 Ceramic yield: It is used to know the quantity of PDC synthesized from
PHMS and also to examine the efficiency of PDC route.
 Stability of PDC and mechanical properties: These properties can be used to
know the quality of PDC produced and applications where PDCs can be used.
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CHAPTER 6
CONCLUSION
From this study following conclusions can be drawn

 The ceramic foams can be synthesized using PU foam scaffolds.

 PDC route can be used to synthesize ceramics.
 Pyrolysis temperature below 600℃ cannot be used to synthesize PDCs.
 The ceramic yield of nearly 70% can be obtained through PDC route.
 Pyrolysis temperature has a significant influence on ceramic’s density, strength
and toughness,
 Optimum mechanical properties depend on both pyrolysis temperature and
duration. These properties peak at 2hrs of pyrolysis.
 The PDC foam shows excellent high temperature stability.

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CHAPTER 7
FUTURE WORK
 The functional properties like electrical and thermal conductivity need to be
explored.
 Microstructural investigation needs to be extended to Transmission
microscopy to understand the mechanism of mechanical behavior.
 PDC’s can be synthesized using different organosilicon polymers and their
properties need to be studied for specific applications.
 Effect of scaffold structure and density can be further explored using various
grades of PU foams.
 Currently pristine ceramics are synthesized, experiment can be continued on
by adding metallic powders, nano fibers or fillers with higher melting point to
the precursor polymer and their properties can be explored.

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CHAPTER 8
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