CHARACTERIZATION OF FIBER OPTIC SENSOR FOR

CORROSION MONITORING

NOOR A’IN BT A.RAHMAN

NOVEMBER 2011

iv 

 

 

 

CHARACTERIZATION OF FIBER OPTIC SENSOR FOR

CORROSION MONITORING

NOOR A’IN BT A.RAHMAN

A thesis submitted in fulfilment of the

requirements for the award of the degree of

Master of Science (Physics)

Faculty of Science

Universiti Teknologi Malaysia

NOVEMBER 2011

vi 

 

Special dedication for my beloved family, mak, abah, boloy, engkis, embo,

along, kakak, ipan, doshi, eman, nomey, and uzair. May Allah shower

his blessings to all of us forever.

Amin.

vii 

 

ACKNOWLEDGEMENT

In the name of Allah, the Most Beneficent and the Most Merciful for the

opportunity and strength to finish this work.

I would like to dedicate special and grateful thanks to my supervisors, Dr.

Asiah Binti Yahaya and Profesor Dr. Rosly Bin Abd. Rahman for their valuables

advice, continuous support and guidance in this work. I would like to thank all

laboratory assistants, technicians, the science officer and all parties who assisted

me during this work.

Deepest thanks to my family and friends for their understanding, love and

encouragement which is very valuable.

viii 

 

ABSTRACT

This research was conducted to characterize the parameter that can be associated

with corrosion activity of metals using fiber optics as sensor. Three samples of metal

rods were selected namely iron, copper and aluminium. Unclad multimode fiber optics

were strapped onto the metal and soaked in corrosive solution. The corrosion process

was monitored by a spectrometer linked to a computer. Two measurement techniques

were used in this research namely transmission and reflection. For transmission

technique, the changes in the intensity spectrum of light from a white LED source after

passing through the unclad region (corrosion activity region) at different exposure

period were monitored. For reflection technique, a Y-probe fiber bundle was used to

observe the reflected intensity from the corroded region. The changes in colour of the

corrosion product had an effect on the reflected component from the light source. The

changes in the intensity spectrum for both techniques were monitored at certain time

intervals. Generally the result showed a reduction in the intensity level with exposure

duration for both techniques but fluctuations also occurred at some exposures. This is

thought to be due to the nature of the corrosion process itself. When the ratios of the

intensities peaks were plotted with exposure, a very distinct drop in the value for iron

occurred for both the reflection and transmission spectra from around days 37 to 44.

This was the period where corrosion activity actually started. After that period, the

value began to level off for reflection measurement but slowly increased for

transmission measurement. For copper and aluminium, the intensity ratios from the

reflected spectrum indicated a more gradual drop. These proved that they were more

resistant to corrosion compared to iron. It seemed that the ratio of the peaks from the

intensity spectrum was the parameter suitable to be associated with the onset of the

corrosion activity of iron.

ix 

 

ABSTRAK

Penyelidikan ini telah dijalankan untuk mencirikan parameter yang boleh

dikaitkan dengan aktiviti kakisan logam yang menggunakan gentian optik sebagai

pengesan. Tiga sampel rod logam telah dipilih iaitu besi, kuprum dan aluminium.

Gentian optik jenis mod berbilang tidak berlapis diikat ke atas logam dan direndam di

dalam larutan menghakis. Proses kakisan telah dipantau oleh spektrometer yang

disambungkan dengan komputer. Dua teknik pengukuran yang digunakan dalam

penyelidikan ini ialah penghantaran dan pantulan. Bagi teknik penghantaran, perubahan

dalam spektrum keamatan cahaya dari sumber LED putih selepas melalui kawasan

tidak berlapis (kawasan aktiviti kakisan) dipantau dalam tempoh pendedahan yang

berbeza. Bagi teknik pantulan, gentian optik berbentuk-Y telah digunakan untuk

memantau keamatan pantulan dari kawasan kakisan. Perubahan warna hasil kakisan

mempunyai kesan ke atas komponen pantulan oleh sumber cahaya. Perubahan spektrum

keamatan bagi kedua-dua teknik dipantau pada sela masa yang tertentu. Umumnya,

hasil menunjukkan penurunan tahap keamatan dengan tempoh pendedahan untuk

kedua-dua teknik tetapi fluktuasi juga boleh berlaku di beberapa waktu tertentu. Ini

adalah kerana sifat proses kakisan itu sendiri. Apabila nisbah puncak keamatan

diplotkan dengan waktu dedahan, penurunan nilai yang sangat berbeza untuk besi

berlaku bagi kedua-dua pantulan dan spektra penghantaran sekitar hari 37 hingga 44.

Ini adalah tempoh di mana aktiviti kakisan telah bermula. Selepas tempoh itu, nilai

tersebut mula menurun ke tahap rendah bagi pengukuran pantulan tetapi menunjukkan

peningkatan perlahan bagi pengukuran penghantaran. Bagi kuprum dan aluminium,

nisbah keamatan daripada spektra pantulan menunjukkan penurunan secara beransur-

ansur. Ini membuktikan bahawa mereka lebih tahan kakisan berbanding besi. Hal ini

menunjukkan bahawa nisbah puncak dari spektrum keamatan adalah parameter yang

sesuai untuk dikaitkan dengan bermulanya aktiviti kakisan bagi besi.

x 

 

TABLE OF CONTENTS

CHAPTER TITLE PAGE

DECLARATION ii

DEDICATION iii

ACKNOWLEDGEMENT iv

ABSTRACT v

ABSTRAK vi

TABLE OF CONTENTS vii

LIST OF TABLES xi

LIST OF FIGURES xii

LIST OF SYMBOLS xv

LIST OF ABBREVIATIONS xvi

LIST OF APPENDICES xvii

1 INTRODUCTION 1

1.0 Background of Study 1

1.1 Statement of Problem 2

1.2 Objectives of Research 3

1.3 Scope of Investigation 3

2 LITERATURE REVIEW 4

2.0 Introduction 4

2.1 Corrosion of Metals 5

2.1.1 Aluminium 8

xi 

 

2.1.2 Copper 10

2.1.3 Iron 11

2.2 Fiber Optic Technology 12

2.3 Work Relating Fiber Optics and Corrosion Measurement 14

2.4 Advantages and Disadvantages of Optical Fiber 21

2.5 The System to be Developed 22

2.5.1 Light Source 22

2.5.2 Unclad Optical Fiber 24

2.5.3 Detector 24

3 RESEARCH METHODOLOGY 25

3.0 Introduction 25

3.1 Preparation the Unclad Optical Fiber 26

3.2 Determination of Length of Unclad Optical Fiber 28

3.3 Metals Samples Preparation 29

3.4 The Laboratory Environment 30

3.5 Seawater Environment 33

3.6 The Measurement System 33

3.7 Light Source 35

3.8 Detector 36

3.9 Methods of Analysis 37

3.9.1 Visual Inspection 38

3.9.2 Direct Transmission Spectrum 38

3.9.3 Reflection Spectrum 39

3.10 Preliminary Study 40

3.11 Control Experiment 44

4 RESULT AND DISCUSSION 46

4.0 Introduction 46

4.1 Experimental Design Result 47

xii 

 

4.1.1 Determination of Length of Unclad Optical Fiber 47

4.1.2 Determination of The Optimum Distance for Reflection

Measurement 49

4.1.3 Result of The Different Jelly Coloured 50

4.1.4 Result of Relation Between Voltage Supply and Intensity Ratio 51

4.1.5 Control Experiment 52

PART I : 53

4.2 Visual Inspection 53

4.2.1 Iron 54

4.2.2 Aluminium 55

4.2.3 Copper 56

4.3 Transmission Spectrum Analysis 57

4.4 Absorbance Profile 60

4.5 Reflection Spectrum Analysis 62

PART II : 66

4.5 Visual Inspection 67

4.5.1 Iron 67

4.5.2 Aluminium 68

4.5.3 Copper 69

4.7 Transmission Spectrum Profile 70

4.8 Absorption Profile 72

4.9 Reflection Spectrum Analysis 73

4.10 Summary 75

5 CONCLUSION AND RECOMMENDATIONS 80

5.0 Introduction 80

5.1 Recommendation 82

xiii 

 

REFERENCES 83

Appendices A-J 90 – 103

PAPERS & PRESENTATION 104

xiv 

 

LIST OF TABLES

TABLE NO. TITLE PAGE

2.1 Types of Corrosion 7

xv 

 

LIST OF FIGURES

FIGURE NO. TITLE PAGE

2.1 Generalized illustration of pitting corrosion on Al

alloys 9

2.2 Fiber optic structures 13

2.3 Experimental set-up 14

2.4 Corrosion activity of reinforced rod using optical

fiber 17

2.5 The metallized of the unclad optical fiber 18

2.6 Transducer schematics showing an input bean

entering at a specific incidence angle 19

2.7 Corrosion process finally breaks the plastic clad

silica fiber 20

3.1 Unclad optical fiber 26

3.2 Three different grades of lapping films 27

3.3 Transmission of light 28

3.4 Length for unclad test 29

3.5 The samples 30

3.6 Q-cyclic Corrosion Chamber 31

3.7 Humidity Cycle in the chamber 31

3.8 Fog function in the chamber 32

3.9 Flow chat to operate the Q-Fog Cyclic

Corrosion Tester Machine 32

3.10 The metals (a) Al, (b) Fe and (c) Cu 33

xvi 

 

3.11 The samples placed in the black cover 34

3.12 Direct method experimental set-up 34

3.13 Modified SMA connector 34

3.14 Reflection measurement set-up 35

3.15 LED transmission spectrum 36

3.16 USB2000 Ocean Optic Spectrometer 37

3.17 LED Intensity spectrum profile from the

spectrometer 39

3.18 Flow chat 42

3.19 Conversion curve 43

4.1 Intensity spectrum in red coloured solution 47

4.2 Intensity spectrum in green coloured solution 47

4.3 Intensity spectrum in blue coloured solution 48

4.4 Power response to sample-detector distance 49

4.5 The reflected intensity spectrum 50

4.6 Intensity spectrum profile 51

4.7 A constant relation of the intensity ratio 52

4.8 Intensity spectrum for transmission of before

and after soaked in 5% NaCl 53

4.9 The appearance of the different stages for Fe 54

4.10 The appearance of the different stages for Al 55

4.11 The photos of corrosion product of Cu 56

4.12 Fe Intensity spectrum 58

4.13 Al Intensity spectrum 58

4.14 Cu Intensity spectrums 59

4.15 Peak intensity ratio at various exposures 59

4.16 Absorbance profiles for all test samples 62

4.17 Fe reflection intensity spectrum 63

4.18 Cu reflection intensity spectrum 64

4.19 Al intensity profile of reflection 64

xvii 

 

4.20 Peak Intensity ratios for reflectance spectrum 65

4.21 The appearance of corrosion product for Fe 67

4.22 The appearance of corrosion product for Al 68

4.23 The appearance of corrosion product for Cu 70

4.24 Fe transmitted Intensity spectrum 70

4.25 Cu transmitted Intensity spectrum 70

4.26 Al transmitted Intensity spectrums 71

4.27 Peak Intensity ratios for reflectance spectrum 71

4.28 Absorbance profile for every test sample 72

4.29 Fe reflection spectrum profile 73

4.30 Cu reflection spectrum profile 74

4.31 Al reflection spectrum profile 74

4.32 Intensity ratio of reflectance spectrum for all test

samples 75

4.33 The unclad fiber before and after undergoing

corrosion process 78

4.34 FESEM photograph for seawater after 100 days 79

xviii 

 

LIST OF SYMBOLS

Al - Aluminium

A - Absorbance

Cu - Copper

Cl- - Chloride ion

D, d - Diameter

Fe - Iron

F - Force

g - Gravity = 9.81 m/s

H+ - Hydrogen ion

l - Length

MP - Megapixels

NaCl - Sodium Chloride

P - Power

PCS - Plastic clad silica

P0 - Output power

Q - Volumetric flow-rate

% - Percentage

xix 

 

%T - Transmission percentages

n - Refractive index

c - Speed of light

v - Velocity

xx 

 

ABBREVIATIONS

EDX - Energy Dispersive X-ray

FBG - Fiber Bragg Grating

FESEM - Field Emission Scanning Electron Microscope

LED - Light Emitting Diode

MMF - Multimode Fiber

SMF - Single Mode Fiber

SMA - Subminiature Type A

xxi 

 

LIST OF APPENDICES

APPENDIX NO: TITLE PAGE

A EDX result for all metals 90

B Area under spectrum and power values 93

C Wavelength values for every voltage supply of LED 94

D Power and area under spectrum graph 95

E Input power for measurement 96

F Intensity ratio for metals in seawater 97

G Output power, transmission and absorbance for metals in seawater 98

H Intensity ratio for metals in laboratory environment 99

I Output power, transmission, and absorbance for metals in laboratory environment 100

J EDX result in seawater environment for all metals 101

1  

CHAPTER 1

INTRODUCTION

1.0 Background of Study

Corrosion occurs through the deterioration of a material or its properties

because of the reaction with the environment. It influences the economic cost and

also creates safety awareness from the damages such as in pipelines, building,

bridges, wastewater system, and even our residence. A recent study in USA of

industrial sectors, reported that 121 billion USD has been spent annually on

corrosion control methods (Andres M. Cardenas-Valencia et al. 2007). The

fundamental of corrosion must be well understood in order to avoid or to remedy the

problem at an earlier stage. Earlier detection can be taken to identify the problem

before it gets too late. Several methods for the diagnosis, detection and measurement

of corrosion in structures are available, but there is no consensus regarding which

method assesses corrosion levels of structures most accurately, that is why the

technique for corrosion detection will remain as an issue and progressing no matter

how corrosion inhibition is being carried out. The feasibility of an optical fiber as

corrosion sensor depends on several advantages which might not be present in others

sensor. Recently, the feasibility of fiber optic as corrosion sensor had been explored

by many researchers from entire world and it became a very interesting field to

study.

 

2  

The revolutions in optoelectronic industries have enabled the development of

fiber optic sensors that offer a series of advantages over conventional electronic

sensors (Siaw, 2003). This development, in combination with advances in the

composite material technology, has opened up the new field of fiber optic sensor in

many field of application to the world. The optical fiber is a very versatile

transmission medium and the advantages of the optical fiber explain why it has

become such an attractive alternation to conventional transmission (Keigo Lizuka,

2009). By dealing with a simple monitoring system and the basic function, it can

function as a good sensor. In recent years, optical fiber sensors have attracted

substantial attention and shown to be capable of monitoring a wide range of physical

measurement in non-destructive technique. The ability of the evanescent field to

interact with the corrosion product on the fiber core has been investigated by

numerous researchers.

1.1 Statement of Problem

The realization of how serious the corrosion impact on our environmental and

economic issue and also the rapid growth of fiber optic sensor technology is the

reason why this works is carried out. At present, several non-destructive methods of

monitoring corrosion activity using fiber optics are available. Most of them proved to

be sensitive for their environments involved but in terms of the sensor preparation or

fiber modification, they could get rather tedious and complicated. In this work,

another approach is being looked into to see the viability of producing a simple and

direct-measurement fiber sensor for measuring corrosion activity of metals. Certain

parameter need to be characterized in this work. In terms of sensor preparation, the

sensor is just the unclad portion of an optical fiber which will be exposed together

with the metals undergoing corrosion. This region must be sensitive enough to detect

any changes in the metals surface due to corrosion activity through its transmitted

and reflected intensities.

3  

1.2 Objectives of Research

The main objectives are to develop:

i. To develop a simple and direct-measurement fiber sensor for

corrosion of metals.

• Characterize the transmitted and reflected intensity spectrum

• Find the other intensity related parameter that can be

associated with corrosion activity

• To relate the intensity to the degree of corrosion of metals in

seawater environment.

1.3 Scope of Study

The scope of this work is to use an unclad optical fiber to characterize the

fiber optic sensor for corrosion studies. A similar environment is also created in a

corrosion chamber in the laboratory. Corrosion of the three metal samples which are

iron, copper and aluminium will also be conducted in this environment to see the

changes if any in the two environments (seawater and laboratory).

Corrosion activity is monitored using spectrometer and the spectrum is

displayed on the computer. The parameter observed in this work is the intensity from

a broad band source in the form of a white phosphor-based Light Emitting Diode

(LED). The characteristic intensity spectrum of the light source featuring two

intensity peaks is monitored for any changes throughout the corrosion activity. In this

work, both the transmitted intensity and the reflected intensity spectrum from the

corrosion region are monitored. Changes in the intensity levels, peak intensity ratios

and wavelength shift are monitored to see if these phenomena could be related to the

stages of corrosion activity of the metals.

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