The effects of stainless steel on the properties of graphite-polypropylene composite for bipolar plate.

SUPERVISOR DECLARATION

" I declare that I have read this thesis and in my opinion this report is sufficient in terms
of scope and qua I ity for the award of the degree of Bachelor of Mechanical Engineering
(Structure & Materials)"

セ@

.............. .

Signature

: ......

Supervisor

: DR. MOHD ZULKEFLI BIN SELA MAT

Date

: 28 JUNE 2013

DR. MOHD ZULKEFLI BIN SELAMAT
Pensyarah Kanan
Fakulti Kejuruteraan Mekanikal
Universiti Teknikal Malaysia Melakl

© Universiti Teknikal Malaysia Melaka

THE EFFECT OF STAINLESS STEEL ON THE PROPERTIES OF GRAPHITEPOLYPROPYLENE COMPOSITE FOR BIPOLAR PLATE

FAIRUZ F AZILLAH BINTI SHUIIlMI

This report is submitted to Faculty of Mechanical Engineering as a
requirements to get award of
Degree of Mechanical Engineering ( Structure & Material)

Faculty of Mechanical Engineering
Universiti Teknikal Malaysia Melaka

JUNE2013


© Universiti Teknikal Malaysia Melaka

ii

DECLARATION

"I hereby declare that the work in this report is my own except for swnmaries
and quotations which have been duly acknowledgment."

セ@

..

:

Signature

: .........

.... ........ ...... .


Author

: FAIRUZ FAZILLAH BINTI SHUHIMI

Date

: 28 JUNE 2013

© Universiti Teknikal Malaysia Melaka

iii

ACKNOWLEDGEMENT

Assalamualaikum w.b.t

Very grateful to Allah S.W.T because of Allah' s endowment, I can execute this
Final Year Project 1 report at the right time. I would like to take this opportunity to
express my deepest heartfelt and thank to all those who have guided and supported me

during my Final Year Project either directly or indirectly.
First of all I would like to thank GOD for this opportunity, and to my parents and
siblings for their love and support. I would like to thank Dr. Mohd Zulkefli bin Selamat
as supervisor, Mr Mohd Syakir bin Ahmad as him assistant researcher and all lecturers
with respect to their direction, guidance, assistance and unselfish support. Special thanks
to my nice appreciation to panels during presentation, Dr. Mohd Fadzli bin Abdollah,
Dr.Olawale Friday, Mr. Omar bin Bapokutty for their valuable advice and nice support
on behalf of me to satisfy this project. Also thanks to all the technicians and staffs from
Department of Mechanical Engineering for their instruction, continuous support and
supervision.

Finally, I would also like to thank those individuals who have contribute to the
success of my training and whose name are not mentioned. They may be my family
members, other FKM staff, friends, and individuals I meet during project progress.
Thank you for all the support and contribution for the success of my Final Year Project
at Universiti Teknikal Malaysia Melaka.

© Universiti Teknikal Malaysia Melaka

iv


ABSTRACT

Over the past decade, rapid progress has been made in the understanding and
development of Conductive Polymer Composites (CPC) as conducting materials. This
project is aimed to study the effects of stainless steel (St) loading on the electrical and
mechanical properties of Graphite (G)/ Stainless steel (St)/ polypropylene (PP)
composite of bipolar plates for polymer electrolyte membrane fuel cells (PEMFC). St is
selected as second filler because it offers good electrical conductivity, high bulk thermal
conductivities, good corrosion resistance and constant particle shape. The analysis of the
G/St/PP composites ratio and the properties of G, St and PP together with the impact of
Graphite (G) as a main filler and Stainless Steel (St) as second filler whereas
polypropylene (PP) as a binder has been carry out. The impact of fillers on the
composite properties was evaluated as well as the ratio of the weight percentage (wt%)
of the composite with 80% for multi-filler material and 20% binder material. The St wt
% is vary from 5 wt % up to 30 wt % of total wt % of multi-filler materials. After
formation of composite through compression molding, the effects of St in G/St/PP
composite have been determined through various tests such as electrical conductivity,
flexure strength, density and hardness before can be used as composition of G/St/PP
composite for bipolar plate. The result showed the analysis for Flexural Strength, Bulk

Density and Shore Hardness meet the required characteristics of bipolar plate as in the
Department of Energy (DOE). But for electrical conductivity, the results showed a very
slight increase which is less than 1OOS/cm.

© Universiti Teknikal Malaysia Melaka

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ABSTRAK

Lebih sedekad yang lalu, kemajuan pesat telah dibuat dalam memahami dan
pembangunan konduktif Polimer Komposit (CPC) yang mengendalikan bahan-bahan.
Projek ini bertujuan untuk mengkaji kesan daripada keluli tahan karat (St) pada sifatsifat elektrik dan mekanikal Grafit (G) I keluli tahan karat (St) I polipropilena (PP)
komposit plat dwikutub bagi polimer elektrolit sel bahan api membran. St dipilih sebagai
pengisi kedua kerana ia menawarkan kekonduksian elektrik yang baik, konduktiviti haba
yang tinggi, ketahanan kakisan yang baik dan bentuk zarah yang berterusan. Analisis
nisbah komposit G I St I PP dan sifat-sifat G, St PP dan bersama-sama dengan kesan
Grafit (G) sebagai pengisi utama dan keluli tahan karat (St) sebagai pengisi kedua
manakala polipropilena (PP) sebagai pengikat telah menjalankan. Kesan pengisi pada
sifat-sifat komposit telah dinilai serta nisbah peratusan berat (% berat) dengan 80%

untuk bahan pelbagai pengisi dan 20% bahan pengikat. Berat St°/o yang berbeza-beza
dari 5% sehingga 30% daripada jumlah berat bahan pelbagai pengisi. Selepas
pembentukan komposit melalui pengacuan mampatan, kesan St dalam G I St I PP
komposit telah ditentukan melalui pelbagai ujian seperti kekonduksian elektrik,
kekuatan lenturan, kepadatan dan kekerasan sebelum boleh digunakan sebagai
komposisi G I St I PP gubahan plat dwikutub. Hasilnya menunjukkan analisis untuk
kekuatan lenturan, ketumpatan dan kekerasan memenuhi ciri-ciri yang diperlukan plat
dwikutub oleh Jabatan Tenaga. Tetapi bagi kekonduksian elektrik, keputusan
menunjukkan peningkatan yang sangat sedikit iaitu kurang daripada 1OOS/cm.

© Universiti Teknikal Malaysia Melaka

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CONTENT

CHAPTER

TITLE


PAGES

TITLE PAGE

CHAPTER I

DECLARATION

11

ACKNOWLEDGEMENT

lll

ABSTRACT

iv

ABSTRAK


v

CONTENT

vi-ix

LIST OF FIGURE

X-Xl

LIST OF TABLE

XU

LIST OF APPENDIX

xiii

LIST OF SYMBOLS


xiv

LIST OF ABBREVIATION

xv

INTRODUCTION
1.1

BACKGROUND
1.1.1

1

Proton exchange membrane
fuel cell

3

1. I .1.1 Polymer Electrolyte

Membrane Fuel Cell

1.1.2

Operation

4

Component of PEMFC

5

1.1 .2.1 Membrane Electrolyte
Assembly (MEA)

© Universiti Teknikal Malaysia Melaka

7

vii

1.1.2.2 Catalysts

CHAPTER2

8

1.2

OBJECTIVE

8

1.3

SCOPE OF STUDY

9

1.4

PROBLEM STATEMENT

9

LITERATURE REVIEW
2.1

CONDUCTIVE POLYMER
COMPOSITES

10

2.1.1 Conductively Filled Polymers

11

2.1.2 Polymers Filled with Conductive

12

Solids
2.2

BIPOLAR PLATE MATERIALS
2.2.1

2.2.2

15

Filler
2.2.1. l Graphite

15

2.2.1.2Stainless Steel

19

Binder
2.2.2.1 Polypropylene

2.3

14

23
23

FABRICATION OF BIPOLAR PLATE

25

2.3.1

Injection Molding

25

2.3.1.1 Equipment

26

2.3.1.2 Power Requirements

26

Compression Molding

27

2.3.2.1 Basic Process of

27

2.3.2

Compression Molqing

2.4

2.3.2.2 Advantages

28

2.3.2.3 Disadvantage

28

TESTING METHOD

29

2.4.1

Electrical Properties

29

2.4.2

Mechanical Properties

30

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CHAPTER3

METHODOLOGY
3.1

CHAPTER4

CHARACTERIZATION OF
RAW MATERI.AL

33

3.2

PRE-MIXING

35

3.3

MELT COMPOUNDING

36

3.4

CRUSH AND PULVERIZE

37

3.5

COMPRESSION MOLDING

38

3.6

TESTING
3.6.1

Electrical Properties

3.6.2

Mechanical Properties
3.6.2.1 Flexural Testing

42

3.6.2.2 Bulk Density Testing

43

3.6.2.3 Shore Hardness Testing

43

RESULT AND ANALYSIS
4.1

ELECTRICAL CONDUCTIVITY
TEST RESULT
4.1.1

44

Determination of Electrical
Conductivity

CHAPTERS

41

45

4.2

FLEXURAL TEST

47

4.3

BULK DENSITY

48

4.4

SHORE HARDNESS

49

DISCUSSION
5.1

DISCUSSION OF RESULT
5.1.1

Electrical Conductivity Testing

51

5.1.2

Flexural Testing

52

5.1.3

Bulk Density Testing

52

5.1.4

Shore Hardness Testing

53

© Universiti Teknikal Malaysia Melaka

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5.2

DISCUSSION OF PROBLEM
ENCOUNTERED
5.2.1

Materials flows out of the mold

54

5.2.2

Material attached to the mold

54

5.2.3

Mold plate loose

55

5.2.4

Surface of sample not uniform
and broken

5.3

CHAPTER6

SOLUTIONS

55
56

CONCLUSION AND RECOMMENDATION
6.1

CONCLUSION

57

6.2

RECOMMENDATION

58

REFERENCES

59

BIBLIOGRAPHY

65

APPENDIX

67

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x

LIST OF FIGURE

BIL

TITLE

PAGE

Figure I.I

Fuel cell

2

Figure I.2

Polymer Electrolyte Membrane Fuel Cell (PEMFC)

3

Figure I.3

Operation of PEMFC

4

Figure I.4

The illustration of components of PEMFC

5

Figure I.5

Bipolar Plates

6

Figure 2.I

Dependence of composite conductivity on the volume

I2

fraction of conductive fillers
Figure 2.2

Schematic representation of conductive particles dispersed 13
in a polymer matrix at different particle volume fractions

Figure 2.3

Classification of materials for BPs used in PEM fuel cells

I4

Figure 2.4

Graphite Specimen

I6

Figure 2.5

Graphite Unit Cell

I7

Figure 2.6

Stainless steel AISI 3I6 (Fe/CrI8/NilO/Mo3)

20

Figure 2.7

Polypropylene

23

Figure 2.8

Chemical structures for polypropylene

23

Figure 2.9

Injection Molding Machine

25

Figure 2.IO

Jandel Four Point Probe

29

Figure 2.I I

Zwick Shore hardness tester and flexural testing machine

30

Figure 2.I2

Density Meter Tester

30

Figure 3.I

Flow Chart Methodology

32

Figure 3.2

Powder of material (a) G, (b) St and (c) PP

33

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Figure 3.3

Measured the weight of graphite and stainless

34

steel due the percentage
Figure 3.4

Ball Mill machine

35

Figure 3.5

Steel Ball

35

Figure 3.6

Measure the weight of St/G and PP

36

Figure 3.7

Internal Mixer Machine

36

Figure 3.8

Outcomes from Internal Mixer Machine (St/GIPP)

37

Figure 3.9

Crusher machine

37

Figure 3.10

Outcomes of crusher process

37

Figure 3.11

Centrifugal Mill machine

38

Figure 3.12

Outcomes of pulverize process

38

Figure 3.13

Four-Point Probe Tester

41

Figure 3.14

Cutter machine

42

Figure 3.15

Standard sizes for Flexural

42

Figure 3.16

Three Point Flexural Test

42

Figure 3.17

Setting the sample to the supporting span

42

Figure 3.18

Electronic Densimeter

43

Figure 3.19

Standard size for density test

43

Figure 3.20

Digital Shore Hardness

43

Figure 4.1

Graph of conductivity versus St wt%

45

Figure 4.2

Graph of flexural strength versus St wt%

47

Figure 4.3

Graph of Density versus St wt.%

48

Figure 4.4

Graph of shore hardness versus St wt%

49

Figure 5.1

Materials flow out of the mold

54

Figure 5.2

Material attached to the mold

54

Figure 5.3

Mold plate loose

55

Figure 5.4

Surface of sample broken

55

Figure 5.5

Mold plate sprayed with lubricant oil

56

© Universiti Teknikal Malaysia Melaka

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LIST OFTABLE

BIL

TITLE

PAGE

Table 2.1

Principal property of filler

16

Table 2.2

Composition ranges for 316L stainless steel

22

Table 2.3

Mechanical properties of 316L stainless steel

22

Table 2.4

Typical physical properties for 316L grade
stainless steels

22

Table 2.5

Properties of polypropylene

24

Table 2.6

The power requirement of injection molding by

26

different material
Table 3.1

Raw material properties of G/St/PP

33

Table 3.2

Composition based on weight percentages

34

Table 4.1

Average result for Conductivity of St/GIPP

45

Table 4.2

Data from top and bottom of composite 20% St

45

Table 4.3

Average result for Flexural Strength of St/GIPP

47

Table 4.4

Bulk Density of St/GIPP

48

Table 4.5

Shore hardness St/GIPP

48

Table 5.1

U.S Department of Energy (US DOE)

51

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LIST OF APPENDIX

BIL

TITLE

PAGE

A

FLOW CHART OF STUDY

67

B

GANTT CHART FINAL YEAR PROJECT 1 & 2

68

c

ASTM C611 ELECTRICAL RESISTIVITY

69

D

ASTM D790-03 FLEXURAL TEST

71

E

ASTM C559-90 BULK DENSITY

77

F

ASTM C886-98 HARDNESS

78

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LIST OF SYMBOL

PEMFC

= Proton Exchange Membrane Fuel Cell I Polymer Electrolyte
Membrane Fuel Cell

PEM

= Polymer Electrolyte Membrane

BPs

= Bipolar Plate

DC

= Direct Current

H20

=Hydrogen

02

=Oxygen

MEA

= Membrane Electrolyte Assembly

G

=Graphite

St

= Stainless Steel

pp

= Polypropylene

PPS

= Polyphenylene sulfide

PVDF

= Polyvinylidene fluoride

CPCs

= Conductive Polymer Composites

IP Cs

= Inherently Conducting Polymers

SPEs

= Solid Polymer Electrolytes

Cr

= Chromium

Ni

=Nickel

Mo

=

LDPE

= Low-Density Polyethylene

HDPE

= High-Density Polyethylene

MFR

= Melt Flow Rate

MFI

= Melt Flow Index

DOE

=US-Department of Energy

Molybdenum

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LIST OF ABBREVIATION

Wt.%

= Weight Percentage

Siem

= Siemens/centimeter

MP a

= Mega Pascal

Cm

= centimeter

µA

= micron Ampere

g/cm 3

= gram/centimeter3

W ·m-

= Watt per metre

µA cm/\ (-2)

=Micro ampere(s) per square centimeter

µm

= micrometer

nm

=nanometer

ncm

= ohm-centimeter

E

=Young's Modulus

mK

= milli Kelvin

oc

= Degree Celsius

© Universiti Teknikal Malaysia Melaka

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CHAPTER 1

INTRODUCTION

1.1

BACKGROUND

One of the maJor factors limiting fuel cell commercialization is the
development of bipolar plates, which are one of PEMFC's key components. Several
types of materials are currently used in bipolar plates, including non-porous graphite
plates, metallic plates with or without coating and a number of composite plates.

The bipolar plate is one of the most important components in a PEM fuel cell.
A polymer composite bipolar plate possessing high strength and high stiffness has been
developed by making use of carbon fiber network in a specific form as the filler
component. The bipolar plates are in weight and volume the major part of PEM fuel cell
stack, and also a significant effect to the stack cost.

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2

Figure 1.1: Fuel cell

So far, many different materials for bipolar plates have been investigated and an
alternative solution consists in polymer composite that combine the process ability and
mechanical properties of the polymeric phase and the conductivity of the carbon fillers.
Both thermo-set resins and thermoplastics were considered and combined to many
different carbon fillers. [ 1]

The interests and limitations of these formulations are presented in terms of
process ability and most relevant properties. A composite material is made by combining
two or more materials to give a unique combination of improved properties, such that
each component retains its physical identity.

In order to improve their commercial liability, many scientific and

technological efforts are being performed on fuel cell systems. On the technical point of
view, bipolar plates should fulfill functional challenges besides ensuring the mechanical
strength of the stack. As a result an optimal material for bipolar plate application should
present an unusual balance of properties, essentially high electrical conductivity and
good mechanical strength.

© Universiti Teknikal Malaysia Melaka

3

1.1.1

Proton exchange membrane fuel cell

Proton exchange membrane fuel cell (PEMFC), also known as polymer
electrolyte membrane (PEM) fuel cells are a type of fuel cell being developed for
transport applications as well as for stationary fuel cell applications and portable fuel
cell applications. Their distinguishing features include lower temperature/pressure
ranges (50 to I 00 °C) and a special polymer electrolyte membrane.

PEMFC are electrochemical devices that convert the chemical energy of
reactants (a fuel and an oxidant) directly to electrical energy in the form of low voltage
direct current (DC) electricity and heat. They have been receiving significant attention
due to their high power density, energy efficiency, and environmentally friendly
characteristics. [2]

Power

End-plate
gos and cooling manifold

Bipolar n ow-rlate
interconnect

- --

Membrane

ャZ・」イッIセc@

sscmbl}

tMEA)

llcat

Figure 1.2: Polymer El ectrolyte Membrane Fuel Cell (PEMFC) [7]

© Universiti Teknikal Malaysia Melaka

4

1.1.1 .1 Polymer Electrolyte Membrane Fuel Cell Operation
I.

Pure hydrogen constantly flows from a simple cylinder containing
compressed hydrogen into the fuel cell and onto the anode it is then split
into hydrogen ions and electrons.

2.

The electrons cannot pass through the electrolyte therefore ; they pass
through the external circuit creating an electric charge.

3.

The electrolyte is sandwiched between the anode and cathode, which 1s
permeable to protons but does not conduct electrons. Hydrogen ions
(protons) permeate across the electrolyte to the cathode. Electrons flow
through an external circuit and provide power.

4.

Oxygen is fed into the fuel cell onto the cathode (positive electrode). The
cathode combines electrons, protons and oxygen to form the by product
which is water. The water then leaves the cell . This is a continuous process
so as hydrogen and oxygen is supplied. [3]

. -. --

Ol (Oxygen)
from Air

HHt(8S"C)
Watu or Air Cool•d

Flow Fi•ld

Plate
セM

Gas Diffusion
Elec:tro