AN ABSTRACT OF A THESIS

METHODS FOR INTRODUCING CONTROLLED POROSITY INTO IM6/3501-6 GRAPHITE FIBER REINFORCED PLASTICS

Richard Eugene Gregory

Master of Science in Mechanical Engineering The introduction of controlled porosity into an IM6/3501-6 composite system was studied. Four methods of introducing porosity were tried and examined with both destructive and nondestructive examination techniques: vacuum pressure variation, microballoons, bag bridging, and AIBN foaming agent. Overall porosity levels from 0.0% to 6% were produced in the samples. Light microscopy and SEM examination were used to determine the void fraction as well as classify the porosity according to shape and location. Mechanical testing was conducted to determine what eects the methods might have on the composites mechanical properties. It was found that for low levels of porosity, the vacuum pressure variation technique was most successful. When higher levels of porosity are desired, the addition of a chemical foaming agent was necessary.

METHODS FOR INTRODUCING CONTROLLED POROSITY INTO IM6/3501-6 GRAPHITE FIBER REINFORCED PLASTICS

A Thesis Presented to the Faculty of the Graduate School Tennessee Technological University by Richard Eugene Gregory

In Partial Fulllment of the Requirements for the Degree MASTER OF SCIENCE Mechanical Engineering

December 2003

CERTIFICATE OF APPROVAL OF THESIS

METHODS FOR INTRODUCING CONTROLLED POROSITY INTO IM6/3501-6 GRAPHITE FIBER REINFORCED PLASTICS by Richard Eugene Gregory Graduate Advisory Committee: Christopher D. Wilson, Chairperson Dale A. Wilson Jiahong Zhu date date date

Approved for the Faculty: Francis Otuonye Associate Vice President for Research and Graduate Studies Date ii

STATEMENT OF PERMISSION TO USE

In presenting this thesis in partial fulllment of the requirements for a Master of Science degree at Tennessee Technological University, I agree that the University Library shall make it available to borrowers under rules of the Library. Brief quotations from this thesis are allowable without special permission, provided that accurate acknowledgment of the source is made. Permission for extensive quotation from or reproduction of this thesis may be granted by my major professor when the proposed use of the material is for scholarly purposes. Any copying or use of the material in this thesis for nancial gain shall not be allowed without my written permission.

Signature Date

iii

DEDICATION

This thesis is dedicated to my wife Kathryn who has been my support and encouragement throughout this ordeal. I owe her big time!

iv

ACKNOWLEDGMENTS

Before I acknowledge anyone else, I must thank God who has blessed me with the opportunity to pursue the things I enjoy. Now for the people God has surrounded me with to make sure I succeeded. First, I would like to thank Dr. Christopher D. Wilson who has been my advisor and mentor for two years now. I have greatly appreciated his help and advice. Also, I would like to thank the other members of my committee, Dr. Dale Wilson and Dr. Jiahong Zhu for their help as well. Next, I would like to thank the TTU Mechanical Engineering Department, the Center for Manufacturing Research, and the National Center for Advanced Manufacturing whose funding made this research possible. I would like to thank my fellow researchers Dr. Darrell Hoy, Dr. Sally Pardue, Dr. Corinne Darvenne, Dr. Joe Richardson, Mike Renfro, Wayne Hawkins, Lance Lowe, Brahmaji Vasantharao, Scott Smith, and Robert Matthews and especially Mark Evans for their assistance with many tasks. I would like to thank Harold Brewer and the late Bob Legg from the Aerostructures Corporation in Nashville, TN. Also, I owe thanks to James Walker at NASA Marshall Space Flight Center in Huntsville, AL. Finally I would like to thank Dr. Phillip A. Allen, without whose support and encouragement I could not have succeeded.

TABLE OF CONTENTS

Page LIST OF TABLES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . LIST OF FIGURES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . LIST OF SYMBOLS Chapter 1. Introduction & Terminology . . . . . . . . . . . . . . . . . . . . . . . . 1.1 Metals vs. Composites . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 1 1 2 3 5 6 7 7 9 9 9 9 9 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . x xi xvi

1.2 What is a Composite Material? 1.3 GFRP Fabrication Methods

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

1.4 GFRP Benets & Applications . . . . . . . . . . . . . . . . . 1.5 GFRP Drawbacks & Weaknesses . . . . . . . . . . . . . . . . 1.6 A Look Ahead . . . . . . . . . . . . . . . . . . . . . . . . . . 2. Problem of Porosity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2.1 Natural Porosity . . . . . . . . . . . . . . . . . . . . . . . . . 2.2 Denitions . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2.2.1 Pore vs. Void . . . . . . . . . . . . . . . . . . . . . . . . 2.2.2 Delamination . . . . . . . . . . . . . . . . . . . . . . . .

2.3 Eects of Porosity on Material Properties . . . . . . . . . . . 2.3.1 Tensile & Compressive Strength . . . . . . . . . . . . . .

vi

vii Appendix 2.3.2 Flexural Strength . . . . . . . . . . . . . . . . . . . . . . 2.3.3 Interlaminar Shear Strength (ILSS) . . . . . . . . . . . . 2.3.4 Fatigue Life . . . . . . . . . . . . . . . . . . . . . . . . . 2.4 Research Objective: Controlled Porosity Introduction 3. . . . . Page 10 11 13 14 16 16 17 17 19 22 23 25 25 26 29 30 32 32 32 33 34

Material & Fabrication . . . . . . . . . . . . . . . . . . . . . . . . . . . 3.1 Raw Material . . . . . . . . . . . . . . . . . . . . . . . . . .

3.2 Double Vacuum Box Process . . . . . . . . . . . . . . . . . . 3.2.1 Process Description . . . . . . . . . . . . . . . . . . . . . 3.2.2 Equipment Description . . . . . . . . . . . . . . . . . . . 3.2.3 Lay-up Process . . . . . . . . . . . . . . . . . . . . . . .

3.3 Controlled Porosity Introduction . . . . . . . . . . . . . . . . 3.3.1 Standard Panels . . . . . . . . . . . . . . . . . . . . . .

3.3.2 Outer Box Pressure Variation . . . . . . . . . . . . . . . 3.3.3 Glass Microballoons 3.3.4 Bag Bridging . . . . . . . . . . . . . . . . . . . .

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

3.3.5 AIBN Foaming Agent 4.

Porosity Measurement Methods & Results 4.1 Porosity Measurement Methods 4.1.1 Density

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

4.1.2 Matrix Digestion

4.1.3 Ultrasonic C-Scan . . . . . . . . . . . . . . . . . . . . . .

viii Appendix 4.1.4 Micrography . . . . . . . . . . . . . . . . . . . . . . . . . 4.2 Porosity Measurement Results . . . . . . . . . . . . . . . . . 4.2.1 Specimen Preparation . . . . . . . . . . . . . . . . . . . Page 36 37 37 38 39 44 50 57 67 67 68 69 70 78 84 84 86 88

4.2.2 Digital Imaging . . . . . . . . . . . . . . . . . . . . . . . 4.2.3 Image Analysis . . . . . . . . . . . . . . . . . . . . . . .

4.2.4 Comparison with C-scan Data . . . . . . . . . . . . . . . 4.2.5 SEM Examination . . . . . . . . . . . . . . . . . . . . . . . . .

4.2.6 Pore Characterization and Measurement in SEM 5. Material Testing Methods & Results

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

5.1 Equipment Description . . . . . . . . . . . . . . . . . . . . . 5.2 Material Characterization 5.3 Tensile Testing . . . . . . . . . . . . . . . . . . .

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

5.4 Damage Threshold Test . . . . . . . . . . . . . . . . . . . . . 5.5 Fatigue Testing 6. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

Conclusions & Recommendations 6.1 Summary & Conclusions

6.2 Recommendations For Future Work . . . . . . . . . . . . . . REFERENCES APPENDIX A : TENSILE TEST DATA PLOTS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

93

B: LIST OF PHOTOGRAPHS INCLUDED ON CD . . . . . . . . . . . . . . 104

ix Appendix Page

VITA . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 106

LIST OF TABLES

Table 3.1 4.1 4.2 4.3 5.1 5.2 5.3 5.4 5.5 5.6 Vacuum Pressure Variation Porosity Comparison. Porosity Measurement Results. . . . . . . . . . . . .

Page 26 40 46 58 69 71 73 74 80 81

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

Vacuum Pressure Variation Porosity Comparison.

Specimen Thickness Variation of Middle Two Laminae. . . . . . . . . . Summary of Material Characterization . . . . . . . . . . . . . . . . . .

Summary of Tensile Test Results. . . . . . . . . . . . . . . . . . . . . . Damage Threshold Test Results . . . . . . . . . . . . . . . . . . . . . . C-Scan Results from Damage Threshold Test . . . . . . . . . . . . . . . Fatigue Test Results. . . . . . . . . . . . . . . . . . . . . . . . . . . . . Changes in Stress and Strain from Fiber Misalignment . . . . . . . . .

LIST OF FIGURES

Figure 2.1 2.2 3.1 3.2 3.3 3.4 3.5 3.6 3.7 3.8 3.9 3.10 3.11 3.12 4.1 4.2 4.3 4.4 Naturally Occurring Porosity in Cryogenic Fuel Tank (100) [3] . . . . Naturally Occurring Porosity in Fuel Tank Nose-cone (100) [3] . . . . Degas and Compaction Phases [15] . . . . . . . . . . . . . . . . . . . .

Page 8 8 18 20 21 21 22 24 24 27 28 28 29 30 41 41 42 43

Double Vacuum Box Apparatus . . . . . . . . . . . . . . . . . . . . . . Prestaging Cure Process Timeline . . . . . . . . . . . . . . . . . . . . . Final Cure Process Timeline . . . . . . . . . . . . . . . . . . . . . . . . Alternate Full Cure Cycle Timeline . . . . . . . . . . . . . . . . . . . . Double Vacuum Lay-up Schematic Peel-back View of Bagging Materials . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

Graph of Void Fraction vs. Vacuum Level Sample of microballoons at 800

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

Location of AIBN or Microballoons Insertion During Layup Bag Bridging Technique

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

AIBN Chemical Chain [18] . . . . . . . . . . . . . . . . . . . . . . . . . Inverted Light Microscope Photomicrograph of Panel 35 Inverted Light Microscope Photomicrograph of Panel 51 Inverted Light Microscope Photomicrograph of Panel 54 Inverted Light Microscope Photomicrograph of Panel 57 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

xi

xii Figure 4.5 4.6 4.7 4.8 4.9 4.10 4.11 4.12 4.13 4.14 4.15 4.16 4.17 4.18 4.19 4.20 4.21 4.22 4.23 4.24 Inverted Light Microscope Photomicrograph of Panel 61 Mean Signal Strength Ultrasonic C-Scan of Panel 35 Mean Signal Strength Ultrasonic C-Scan of Panel 51 Mean Signal Strength Ultrasonic C-Scan of Panel 54 Mean Signal Strength Ultrasonic C-Scan of Panel 57 Mean Signal Strength Ultrasonic C-Scan of Panel 55 Mean Signal Strength Ultrasonic C-Scan of Panel 61 SEM Photomicrograph of Panel 35 Laminae Interfaces . . . . . . . . Page 44 45 46 47 48 49 51 52 52 53 54 55 55 56 56 57 58 59 59 60

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

SEM Photomicrograph of Panel 35 Close-up of Laminae Interfaces . . . Photomicrograph of Panel 51 Laminae Interfaces . . . . . . . . . . . . . Photomicrograph of Panel 51 Close-up of Laminae Interfaces . . . . . . Photomicrograph of Panel 54 Laminae Interfaces . . . . . . . . . . . . . Photomicrograph of Panel 54 Close-up of Laminae Interfaces . . . . . . Photomicrograph of Panel 57 Laminae Interfaces . . . . . . . . . . . . . Photomicrograph of Panel 57 Close-up of Laminae Interfaces . . . . . . Photomicrograph of Panel 61 Laminae Interfaces . . . . . . . . . . . . . Photomicrograph of Panel 61 Close-up of Laminae Interfaces . . . . . . Panel 35 Thickness Variation Measurement of Middle Two Laminae . . Panel 51 Thickness Variation Measurement of Middle Two Laminae . . Panel 54 Thickness Variation Measurement of Middle Two Laminae . .

xiii Figure 4.25 4.26 4.27 4.28 4.29 4.30 4.31 4.32 4.33 4.34 4.35 5.1 5.2 5.3 5.4 5.5 5.6 5.7 5.8 5.9 Panel 57 Thickness Variation Measurement of Middle Two Laminae . . Panel 61 Thickness Variation Measurement of Middle Two Laminae . . Representative Round Void in Panel 51 . . . . . . . . . . . . . . . . . . Representative Elliptic Void in Panel 51 . . . . . . . . . . . . . . . . . Page 60 61 62 62 63 64 64 65 65 66 66 68 68 74 74 75 75 75 76 76

Representative Linear Void in Panel 51 . . . . . . . . . . . . . . . . . . Representative Round Void in Panel 61 . . . . . . . . . . . . . . . . . . Representative Elliptic Void in Panel 61 . . . . . . . . . . . . . . . . .

Representative Linear Void in Panel 61 . . . . . . . . . . . . . . . . . . Representative Resin Rich Region in Panel 51 Representative Resin Rich Region in Panel 57 Representative Resin Rich Region in Panel 61 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

MTS Test Frame with Specimen and Extensometer Composite Specimen with E-Glass Tabs

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

Preliminary C-scan of Strip 35-07 . . . . . . . . . . . . . . . . . . . . . Final C-scan of Strip 35-07 . . . . . . . . . . . . . . . . . . . . . . . . . Preliminary C-scan of Strip 51-10 . . . . . . . . . . . . . . . . . . . . . Final C-scan of Strip 51-10 . . . . . . . . . . . . . . . . . . . . . . . . . Preliminary C-scan of Strip 54-09 . . . . . . . . . . . . . . . . . . . . . Final C-scan of Strip 54-09 . . . . . . . . . . . . . . . . . . . . . . . . . Preliminary C-scan of Strip 57-09 . . . . . . . . . . . . . . . . . . . . .

xiv Figure 5.10 5.11 5.12 5.13 5.14 5.15 A.1 A.2 A.3 A.4 A.5 A.6 A.7 A.8 A.9 Final C-scan of Strip 57-09 . . . . . . . . . . . . . . . . . . . . . . . . . Preliminary C-scan of Strip 61-09 . . . . . . . . . . . . . . . . . . . . . Final C-scan of Strip 61-09 . . . . . . . . . . . . . . . . . . . . . . . . . Panels 36 and 37 Fatigue Plot, ult =10600 psi. . . . . . . . . . . . . . . Saw Cut Edge of Composite Specimen Failed Edge of Specimen 37-7 . . . . . . . . . . . . . . . . . . Page 76 77 77 79 82 83 94 94 95 95 96 96 97 97 98 98 99 99

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

Tensile Plot for Specimen 35-1 . . . . . . . . . . . . . . . . . . . . . . . Tensile Plot for Specimen 35-2 . . . . . . . . . . . . . . . . . . . . . . . Tensile Plot for Specimen 35-3 . . . . . . . . . . . . . . . . . . . . . . . Tensile Plot for Specimen 35-4 . . . . . . . . . . . . . . . . . . . . . . . Tensile Plot for Specimen 51-1 . . . . . . . . . . . . . . . . . . . . . . . Tensile Plot for Specimen 51-2 . . . . . . . . . . . . . . . . . . . . . . . Tensile Plot for Specimen 51-3 . . . . . . . . . . . . . . . . . . . . . . . Tensile Plot for Specimen 51-4 . . . . . . . . . . . . . . . . . . . . . . . Tensile Plot for Specimen 54-1 . . . . . . . . . . . . . . . . . . . . . . .

A.10 Tensile Plot for Specimen 54-2 . . . . . . . . . . . . . . . . . . . . . . . A.11 Tensile Plot for Specimen 54-3 . . . . . . . . . . . . . . . . . . . . . . . A.12 Tensile Plot for Specimen 54-4 . . . . . . . . . . . . . . . . . . . . . . .

A.13 Tensile Plot for Specimen 57-1 . . . . . . . . . . . . . . . . . . . . . . . 100 A.14 Tensile Plot for Specimen 57-2 . . . . . . . . . . . . . . . . . . . . . . . 100

xv Figure Page

A.15 Tensile Plot for Specimen 57-3 . . . . . . . . . . . . . . . . . . . . . . . 101 A.16 Tensile Plot for Specimen 57-4 . . . . . . . . . . . . . . . . . . . . . . . 101 A.17 Tensile Plot for Specimen 61-1 . . . . . . . . . . . . . . . . . . . . . . . 102 A.18 Tensile Plot for Specimen 61-2 . . . . . . . . . . . . . . . . . . . . . . . 102 A.19 Tensile Plot for Specimen 61-3 . . . . . . . . . . . . . . . . . . . . . . . 103 A.20 Tensile Plot for Specimen 61-4 . . . . . . . . . . . . . . . . . . . . . . . 103

LIST OF SYMBOLS

Symbol m CMC dg dr g GFRP in Hg Md MMC PMC psi r SEM t1/2 T V Vv Vr Vm

Description micrometer microstrain Ceramic Matrix Composite density of ber density of resin ber, weight % Graphite Fiber Reinforced Composite inches mercury, measure of vacuum measured density of specimen Metal Matrix Composite Polymer Matrix Composite pounds per square inch resin, weight % Scanning Electron Microscope half life in minutes temperature in Kelvin void content, volume % void volume percent in the specimen volume percent of ber in the specimen volume percent of resin in the specimen

xvi

CHAPTER 1 INTRODUCTION & TERMINOLOGY

This chapter will begin with a short discussion contrasting metals and composites. An overview of composite material types will follow along with a discussion of current fabrication methods. Benets and applications and drawbacks and weaknesses of composite materials will be discussed next. Finally, the outline for the following chapters will be given.

1.1 Metals vs. Composites

Metals can be forgiving materials to work with because they are well equipped for dealing with discontinuities. In fact, metals are full of discontinuities. A metal can slip around discontinuities and plastically deform near stress concentrations to relieve stresses. This behavior in the presence of aws is one of the characteristics that makes metals an attractive engineering material for many fracture critical designs. One of the fastest growing groups of materials used in the aerospace industry today are composite materials. Composites materials are fundamentally dierent materials and have a dierent benets and weaknesses. Before that is discussed, an introduction to composite materials is needed.

1.2 What is a Composite Material?

The name composite material is given to many engineering materials used today. Strictly speaking, a composite is any material made up of two or more dierent materials blended to make a new material system with two parts: a matrix material 1

2 and a reinforcing material. In a composite system, the matrix material acts like a binder to hold everything together. The matrix material is usually something that can be molded, cured, or cast easily around the reinforcing material. Cement, resin and molten metals are examples of common matrix materials. The reinforcement material is the part of the system that adds some special characteristic to the matrix, such as increased strength, stiness or dimensional stability. Reinforcement materials can be classied as bers, whiskers, or particles. Carbon bers, glass whiskers, and rocks are examples of common reinforcement materials. Composite material systems can then be divided into three categories: Polymer Matrix Composites (PMC), Ceramic Matrix Composites (CMC), and Metal Matrix Composites (MMC). Examples of each type of system are berglass reinforced plastics (a PMC, resin matrix with glass ber reinforcement), concrete (a CMC, cement matrix with rock particle reinforcement), and aluminum boron (a MMC, aluminum matrix with boron ber or whisker reinforcement). The material studied in this research was a Graphite Fiber Reinforced Plastic (GFRP) which is in the PMC family. Further discussion on composite materials will be limited to GFRPs.

1.3 GFRP Fabrication Methods

All composite manufacturing methods involve some form of mold. A mold is needed because the matrix material is either introduced to the reinforcement as a liquid, or its viscosity decreases greatly during the cure cycle to ensure adequate wetting, or covering, of the reinforcement. Using a mold has the drawback of making the curing process somewhat labor intensive, but the benet of being able to form the composite to the desired shape during the process.

3 There are many dierent methods for fabricating GFRP components. One of the most widely used is an autoclave which uses a combination of elevated temperature and pressure to cure the material. Autoclaves can be used on large and small scales and produces very high quality parts. There are other methods used in industry that have specic applications. Pultrusion is very similar to extrusion processes for metals, except that the composite is pulled through a die instead of pushed. Pultrusion is good for simple straight geometries such as L-shaped or T-shaped brackets. In lament winding, a continuous ber is wrapped around a mandrel to create a nished part. This is widely used for round or spherical parts such as pressure vessels. Resin Transfer Molding (RTM) is similar to injection molding for plastics or metals and uses a die or mold to form the bers and then injects the polymer matrix into the mold to cure. RTM can also be used with a vacuum and is then called Vacuum Assisted Resin Transfer Molding (VARTM). VARTM is used with specic composite systems that use thermosetting resins. A less widely used method in the aerospace industry is the simple vacuum bag cure method. In this process, the composite is cured under a vacuum at elevated temperatures. Vacuum bag curing is used much less because it is dicult to produce a large-scale part with the same quality as an autoclave part.

1.4 GFRP Benets & Applications

Usually, aerospace designers select a GFRP composite to replace a high strength to weight ratio metal such as aluminum, titanium, or magnesium. The success of this choice depends upon the basis of the design, strength, stiness, weight, fracture resistance, etc. Dierent composite systems have dierent strengths and weaknesses

4 and may or may not be suited for a certain type of design. The benets of composite materials vary from one system to the next. In any composite system, the goal is to combine the advantages of the two materials while balancing or reducing their weaknesses. For any composite to be useful, it must have superior properties when compared to the individual materials used separately. Strength and stiness are the rst major advantages of GFRP composite materials. GFRPs possess a relatively high tensile modulus which makes them suitable for applications where high stiness and dimensional stability are required such as airplane wing structures. GFRPs have very high tensile strengths which make them suitable for high stress applications such as pressure vessels. Because of this high stiness and dimensional stability, they can be made to have a near zero coecient of thermal expansion which makes them attractive for cases that involve high temperature gradients such as satellite platforms. GFRPs also have very good fatigue properties. According to Strong [1],

GFRPs can retain as much as 60% of their strength in fatigue applications compared to as little as 10% for some metals. This makes GFRPs a good choice for high stress, long life applications such as helicopter rotor blades. An obvious advantage of GFRPs is weight savings over comparable metallic structures. This weight savings depends heavily on the part geometry and application. Weight savings over a metal structure could range from 5% for supercritical structures to as high as 40% for spacecraft applications according to Jones [2]. In designs where weight is a controlling factor, such as spacecraft, even the smallest weight savings can have tremendous savings later in reduced fuel costs and increased payload capacity. An advantage of composites that is often overlooked is the potential for savings on overall manufacturing and service costs by using a composite material [2]. Since

5 a composite is formed during the curing process, a near-net shape can be produced directly from the mold. Very little machining is required if the initial shape can be molded close to the nal shape. Reduced machining leads to increased material utilization. Therefore, less material is required and less scrap is produced. Composite systems tend to be more expensive when compared to noncomposite alternatives due to higher per-pound material costs. This price increase is usually oset by other savings or justied by some special characteristic that the composite oers. In other cases, the raw material costs of the structure may be higher, but over the life of the part, the total cost may be less due to reduced service requirements or increased life span of the structure.

1.5 GFRP Drawbacks & Weaknesses

While the near-net shape of some composites is an advantage, production rates can be a major disadvantage. Composite manufacturing methods are time intensive and do not lend themselves well to mass production so they cannot produce parts in the quantities required for large scale production. For this reason, composite materials still do not have a strong presence in the automotive industry. One notable exception to this is the use of composites in the sporting equipment industry. Golf clubs, tennis rackets and shing poles are examples of high volume production parts that have been successfully produced with composites. This is mainly due to the simplicity of the part being produced and advances in specialized processing techniques that have reduced overall production times for these applications. GFRPs can be very sensitive to aws and may not behave well in the presence of a aw. This makes fracture mechanics and important consideration when designing

6 with composites. Stress concentrations can severely degrade the performance of the part because GFRP cannot deform plastically to relieve the stresses. Some common aws in GFRP include foreign object matter, kinked or broken bers, and porosity. The behavior of GFRP in the presence of these situations is called damage tolerance and is the driving force behind this research.

1.6 A Look Ahead

In Chapter 2, the focus of this research will be introduced and discussed along with previous work and publications in this eld. Objectives for this research will be discussed at the end of Chapter 2. The fabrication method and porosity introduction methods used in this research will be discussed in Chapter 3. Chapter 4 will discuss the porosity measurement techniques and results. The mechanical tests conducted and their results will be discussed in Chapter 5. Finally, a summary of ndings and recommendations will be presented in Chapter 6.

CHAPTER 2 PROBLEM OF POROSITY

First in this chapter, natural porosity samples will be examined to compare to porosity created later in this research. Next, some terms used in this research will be dened. Previous research will be examined to determine the eects of porosity on the mechanical behavior of GFRPs. Finally, the objectives for this research will be outlined.

2.1 Natural Porosity

Porosity is a naturally occurring phenomena in composite manufacturing processes. Porosity has a variety of causes, such as incorrect curing pressure, and tooling leaks. Figures 2.1 and 2.2 are examples of naturally occurring porosity from some composite structures. These picture were taken by James Walker [3] at NASA Marshall Space Flight Center in Huntsville, AL. These samples are of autoclave cured brous PMC composites. The location of the porosity should be noted here and will be of interest in samples produced in this research. Figure 2.1 is part of a cryogenic fuel tank project for NASA. The porosity in this sample is very large and is aligned along the laminae interfaces. Figure 2.2 is part of the nose-cone for the Space Shuttles external fuel tank. The porosity in this sample is smaller and more round and occurs within the plys, not just at the interfaces. The void fraction in both samples was approximately 12%.

Figure 2.1. Naturally Occurring Porosity in Cryogenic Fuel Tank (100) [3]

Figure 2.2. Naturally Occurring Porosity in Fuel Tank Nose-cone (100) [3]

9 2.2 Denitions

2.2.1 Pore vs. Void

Much of the discussion in this research will center around the occurrence of porosity and sites that will be called pores and voids. Porosity will be used as a general term to describe the occurrence of any gas pockets inside a laminate. Pore and void are used interchangeably in literature and will be so here. However, both terms will be used to describe features that are at least as large as one ber diameter, approximately 4 m.

2.2.2 Delamination

Delamination is the separation of a cured laminate composite along the laminae interface lines. This failure mode eectively splits the laminate into its separate layers. With nothing holding them together, the layers are much weaker by themselves that when they are joined together. Delamination is of interest when discussing porosity because porosity tends to be located at lamina interfaces. Smaller voids can also coalesce during the cure cycle and start behaving like a delamination.

2.3 Eects of Porosity on Material Properties

2.3.1 Tensile & Compressive Strength

Tensile strength is the property that determines or denes a materials ability to withstand uniform tensile loading. Tensile strength is of interest because brous

10 composites have a preferred strength direction and are designed to be loaded in tension whenever possible. With metallic materials, tensile tests are run to determine the materials response and are usually quantied by the yield strength of the material. However, GFRPs do not have a yield strength. Gay et al. [4] explain that for composites, the material response is elastic up to material rupture because the material cannot yield by local plastic deformation as classical metals can. This lack of any plasticity causes the resin matrix and the graphite bers to behave in a brittle manner. Instead, the ultimate strength is used to describe the response of a composite material. Garretts [5] research on manufacturing aws and service damage investigated, among other things, the presence of porosity near a fastener hole. Tests were run in tension and compression with wet and dry specimens with porosity levels ranging from 1% to 5%. Garrett found that the greatest sensitivity was in the wet state in compression where there was a reduction of 12% in compressive strength. For dry tension specimens, there was no change. This indicates that porosity may not be a particularly big problem in simple tensile and compressive loading.

2.3.2 Flexural Strength

Flexural strength is a materials ability to withstand bending loads. This is of interest whenever a composite is formed in an angled or curved section. Flexural strength is also important if the loads on a part change in service to induce bending into a composite part. Grelsson [6] studied the eect of increased porosity levels on material strength and measured the response by a four-point bend test. The dierent porosity levels were manufactured by changing the curing pressure of the laminate in the autoclave

11 to introduce porosity. Porosity levels of 0.0% to 3.1% porosity were produced. Grelsson noted that at higher porosity levels, the individual pores tended to cluster and merge into larger voids that act like small delaminations. His test indicated a pattern of reduced exural strength with increased variation as porosity level increased. Low porosity levels specimens had acceptable strengths. However, the trend was that strength levels were decreasing with increasing porosity. This trend tended to accelerate though as higher porosity levels were tested. Work by Kan et al. [7] focused on molded composite anges. In production parts, it was noticed that porosity tended to occur where curing pressures were nonuniform, such as in the region of a curved section. Specimens were taken from a production part with naturally occurring porosity. The specimens were examined by multiple methods to determine the porosity level and then tested under pure bending conditions. The study suggested that a drop of 30% to 50% in interlaminar tensile strength can occur with high levels of porosity.

2.3.3 Interlaminar Shear Strength (ILSS)

InterLaminar Shear Strength (ILSS) is the ability of a laminated material to resist sliding between individual layers. ILSS mainly aects the matrix because the matrix material is the only part of the composite that supports shear stresses. ILSS can be easily illustrated by a stack of paper. The individual pages slide against each other when shear stresses are applied to the upper and lower boundaries of the stack. ILSS is greatly reduced when voids are present in a laminate because these voids usually occur at the laminae interfaces where the laminate is most susceptible to shear stresses.

12 In some literature, ILSS has been called the Achilles heel of composite materials since shear forces load the weakest part of the composite, the matrix. Pipes [8] submitted short-beam specimens to fatigue loading to determine the reduction in ILSS over the life of the composite. He found that while ber tension possesses an endurance of 80% of the ultimate strength, the ILSS fatigue limit diminished to less than 55% after one million cycles. Research done by Hancox [9] looked at the shear response of composite tubes. Solid composite tubes with varying degrees of porosity were tested in torsion to determine the change in shear modulus and shear strength. Previous studies in this area predicted a drop of 10% to 50% in these properties with void fractions in the 5% range. However, Hancox found a steady reduction in these properties with a 70% reduction at a 5% void fraction which was the limit of his research. Judd and Wright [10] performed a survey of over 47 previous studies into the eects of porosity on mechanical properties of composites. The majority of these studies focused on porosity values between 0.0% and 5%. ILSS was the property most often reviewed in the works and was quantied more completely. From this survey, they determined that there exists a linear decrease in ILSS of 7% per 1% increase in porosity with other properties being aected to a similar extent. This relationship was found to be true regardless of the resin or ber used. There were indications that a more serious drop in ILSS may exist between 0.0% and 1%, but a more accurate method of measuring porosity in needed to conrm this. Yoshida et al. [11] looked at a statistical relationship between ILSS and porosity. It was noted that mechanical reliability of composites decreases with increased porosity. They used a chemical foaming agent to introduce porosity into their specimens for study and veried the void fraction by density measurements. The ILSS

13 of the specimens was measured using the short beam test method per ASTM D2344. Using regression analysis and a t-test, they found a 4% to 7% reduction in ILSS with every 1% increase in porosity.

2.3.4 Fatigue Life

Fatigue life is the ability of a material to withstand repeated loading throughout its life. Typically, GFRPs have very good fatigue properties. As explained by Gay et al. [4], this is because as a crack propagates through a laminate, the stress concentration at the crack tip causes failure in the resin. This failure debonds the bers, which actually causes a relaxation and ends the crack propagation. Once the crack has ended, the damage progression stops until another crack has begun. Dharan [12], found that the main cause for fatigue failures in ber reinforced composites was due to matrix cracking. In these cases, a crack nucleated from the matrix material surrounding the reinforcing bers. The crack then grew similar to a crack in a metal and lead to the eventual failure of the specimen by causing ber failures and eventual interfacial shear failures. Fatigue loading is perhaps where the greatest dierence between porous and nonporous specimens can be seen. As noted by both Gay and Dharan, matrix cracks lead to the failure of composites. These cracks will begin at local stress concentrations and propagate from there. In porous composites, voids could serve as nucleation sites for matrix cracks which would greatly reduce the time needed to start a crack and thereby reducing the fatigue life. In nonporous specimens, this process takes longer because there are not as many discontinuities to serve as crack nucleation sites. Dill et al. [13] performed a study with berglass composites to examine the inuence of porosity on fatigue life. Their specimens were fabricated with varying

14 amounts of porosity by varying the level of the bag vacuum and the autoclave pressure during the cure cycle. Specimens with void fractions of 0.11% to 2.66% were produced by this process and were submitted to static tensile tests and zero-max fatigue tests. They noticed a 10% reduction in tensile strength. They also noticed a reduction in fatigue life of 20% at low stress levels and up to 50% at high stress levels.

2.4 Research Objective: Controlled Porosity Introduction

More research is needed into the behavior of composite materials in the presence of porosity. Such research would benet industry in the disposition of as-built hardware with naturally occurring porosity. Currently, such parts are discarded or reworked when possible. A better understanding of the behavior of GFRP in the presence of porosity would lead to clearer rules for using or disposing of production components with porosity and more accurate design tools for engineers to work with. The NonDestructive Evaluation (NDE) and manufacturing communities would benet from being able to produce composite specimens with controlled amounts of porosity. Standards are needed to use with calibration and training. A well understood and documented method of porosity introduction would assist in the production of such standards. To gain this better understanding or produce such standards, samples must be produced for study. A method of creating porosity in a predictable and repeatable manner is needed to produce these samples. This research will concentrate on evaluating proposed methods and selecting one method to be used in future research. Four methods of porosity introduction will be studied in this research: 1. vacuum pressure variation 2. microballoon introduction

15 3. bag bridging 4. chemical foaming agent introduction.

CHAPTER 3 MATERIAL & FABRICATION

The previous chapter focused on the eects of porosity on the mechanical behavior of GFRPs. This chapter will move on to the fabrication of GFRP samples produced for this research. A description of the manufacturing method will be given followed by an explanation of the four porosity introduction methods.

3.1 Raw Material

The panels fabricated in this study were made of IM6/3501-6, an intermediate modulus (IM6) ber, with a thermoset polymer resin (3501-6). The raw material was a prepreg tape purchased from Cytec Engineered Materials on a 60.75 in. roll. The prepreg had a 63% ber content and had an areal weight of 143.3 g/m2 , commonly referred to as grade 145. The particular pedigree was a formulation made for Bell Helicopter, so much of the information about the resin composition and the ber treatment was not available. The panels made for testing were eight layer laminates, [0/45/90/ 45]S , and were approximately 0.050 in. thick when fully cured. Material properties were obtained from the website of the University of California San Diego Composites and Aerospace Structures Laboratory [14] which were using the same material system, but a dierent processing technique. For this reason, independent material characterization tests were conducted and will be discussed later in Chapter 5.

16

17 3.2 Double Vacuum Box Process

3.2.1 Process Description

An autoclave process has historically been the preferred manufacturing process in the aerospace industry for carbon and graphite ber reinforced plastics. This process uses elevated temperatures and pressures to produce a very high quality, nearly void-free product. However, it requires some very large and expensive equipment, making it impractical for producing very small parts such as those used for research or damage repair applications. Glen Sherwin [15] at The Aerostructures Corporation in Nashville, TN, conducted a research project to investigate a non-autoclave process for producing a partially cured, or staged, composite laminate for use as an in-eld repair patch. A double vacuum out-of-autoclave process was investigated. It employs a conventional vacuum bag to provide the rst vacuum and a steel outer box to provide the second vacuum. The cure cycle is divided into two parts: 1) staging and 2) nal cure. The staging process produces a partially cured laminate that can be fully cured immediately or stored for future use. In either case, the staged laminate can be reheated and formed to the contour of a damaged structure. The nal cure cycle produces a fully cured laminate that is ready for use. The staging process consists of two phases: Degas and Compaction, illustrated in Figure 3.1. In the Degas phase, a vacuum of approximately 27 in. Hg is applied to both the inner vacuum bag and the outer vacuum box to remove any pressure gradient between the two vacuum volumes. The lack of a pressure gradient eectively removes the compacting force of the bag which allows adequate pathways for any gases to freely escape the laminate. The vacuum also draws entrapped gases out of the laminate

18

Figure 3.1. Degas and Compaction Phases [15] instead of pushing it out as an autoclave would do. In the Compaction phase, the outer box is vented to the outside atmosphere and the vacuum is maintained on the inner vacuum bag producing a pressure gradient which applies a force from the bag. This force compacts the layers of the laminate together. Both of these phases are carried out at elevated temperatures to ensure that the viscosity of the resin is low enough so that it will bind the layers together. The temperatures in both phases are kept below the full cure temperature of the matrix system to prevent complete curing of the laminate. Sherwin found that the critical parameters are the dwell temperatures at each stages and the timing for switching from Degas to Compaction. After some experimentation, Sherwin found that the optimal temperature for these phases was related to the viscosity prole of the resin system. The optimal situation was to have the

19 resin reach its minimum viscosity during the staging process to make it more stable during the nal cure cycle in the eld. The viscosity during the nal cure cycle remained high when staging temperatures were high. However, the resins viscosity was required to decrease during nal curing to make the laminate exible enough to be formed to the contour of the structure in the eld. The laminate could then be fully cured in the box apparatus or on the damaged structure using a conventional vacuum bag process. In Sherwins study, the composites produced by this process were evaluated and compared to conventional autoclave-processed laminates. The laminate was inspected using ultrasonic NDE methods and found to be of acceptable quality. A cross-section was then cut from the laminate for microscopic examination and was found to contain virtually no porosity.

3.2.2 Equipment Description

The outer vacuum box, shown in Figure 3.2 was loaned to TTU by The Aerostructures Corporation for this research. It was fabricated out of 1/2 in. steel plate to withstand the stresses created when the vacuum was applied. The lid was reinforced with square tubing to prevent it from distorting under vacuum and breaking the seal with the box. The required rigidity and size, 28 in. 32 in. 9 in., of the vacuum box makes for a very heavy piece of equipment. The box has ports with gauges for both vacuums, along with power connections and thermocouple leads passing though the wall of the box. The thermal energy is supplied by a 120 volt, 20 amp Heatcon heater blanket inside the box controlled by an Omega CN Series temperature controller [16] and an Omega solid state relay outside the box. The controller has multiple dwell, ramp

20

Figure 3.2. Double Vacuum Box Apparatus and soak parameters so that the entire process can be programmed and run as one continuous cycle or run as separate parts, whichever is needed. The stage prole is shown in Figure 3.3, and the nal cure cycle is shown in Figure 3.4. The alternate full cycle is shown in Figure 3.5. All laminates in this study were made with the full cycle option. The vacuums were supplied by two Cenco Hyvac 14 vacuum pumps, which were capable of producing a 27 - 29 in. Hg vacuum depending on the quality of the seal. The pumps were controlled by the operator and had to be powered on and o manually at the appropriate times during the cure cycle. This process could be automated with the addition of a programmable logic circuit.

21

Prestage Cure Timeline 300

250

200 Temperature ( F)

150

100

50

50

100 Time (minutes)

150

200

Figure 3.3. Prestaging Cure Process Timeline

Final Cure Timeline 400

350

300

Temperature ( F)

250

200

150

100

50

50

100

150

200

250 300 Time (minutes)

350

400

450

500

550

Figure 3.4. Final Cure Process Timeline

22
Alternate Full Cycle Timeline 400

350

300

Temperature ( F)

250

200

150

100

50

50

100

150

200 Time (minutes)

250

300

350

400

Figure 3.5. Alternate Full Cure Cycle Timeline 3.2.3 Lay-up Process

The laminate was bagged with several layers and kinds of materials to allow for adequate air removal and resin ow. Figures 3.6 and 3.7 show the dierent layers in the bagging process. The bag and laminate were laid up on a composite-backed honeycomb base plate. This sti base plate was needed so that the system would not warp when the vacuum is applied. The bottom layer was a berglass N10 breather cloth which provides pathways for degassing. Above the N10 cloth, was the heater blanket that supplied the thermal energy for the process. On top of the heater blanket, was a layer of porous teon followed by a layer of non-porous teon. These layers protected the heater blanket from the resin since it runs when its viscosity decreased. A thin aluminum caul sheet was placed next to support the laminate and to give it a better surface nish. An adhesive backed layer of nonporous teon was applied

23 to the aluminum caul sheet to prevent the laminate or run-o resin from bonding to it. Layers of nonporous and porous teon lm were layered above and below the laminate to aide in controlling and facilitating resin run-o. The nonporous layers had a tendency to wrinkle during curing which left impressions in the cured panel. This wrinkling may be caused when the laminate shrunk during curing. This layer did not shrink in the same manner but instead, stuck to the laminate and was wrinkled in the process. No method of eliminating this phenomena was found. A second aluminum caul sheet with adhesive backed nonporous teon was placed on top of these layers between the compaction stage and the nal cure to further compact the laminate in the nal cure and provide a better surface nish on the top surface of the laminate. Another layer of N10 breather cloth was applied on top to allow for degassing. Finally, the vacuum bagging material was applied over the top and was sealed to the base plate with vacuum bag sealant tape. This sealant tape was very sticky and had a putty-like consistency. It had a very high resistance to shear so that it did not smear when the vacuum was applied. A two piece vent base was used to pull the vacuum on the bag. The bottom piece was placed inside the bag and a hose was screwed into it to connect to the vacuum pump.

3.3 Controlled Porosity Introduction

Before discussing panels and samples examined in this research, some explanation is needed of the numbering system for panels, strips, samples, and photographs. Panels in this research were numbered in the order they were made and labeled with a two digit number, such as Panel 35. Strips were then cut from these panels for testing or examination and numbered in the order cut. These strips were designated by the

24

Figure 3.6. Double Vacuum Lay-up Schematic

Figure 3.7. Peel-back View of Bagging Materials

25 panel number followed by the strip number such as strip 35-5. Specimens cut from a strip were numbered as cut and labeled with the panel, strip and specimen number such as specimen 35-5-4. Finally, photographs taken of a specimen were numbered in the order taken and labeled with the panel, strip, specimen, and picture number such as picture 35-5-4-01.

3.3.1 Standard Panels

Before trying to introduce porosity, several panels were made to learn about the manufacturing process. Through this exercise, the quality laminate that could be produced using this process was better understood. As with Sherwins work, these standard panels were found to be virtually free from porosity. The average thickness of this panel was 0.045 in. with a standard deviation of 0.00058 in. measured in 24 locations. All panels were examined using the ultrasonic C-scanning technique after fabrication. The mean signal strength from these scans was used to determine the relative porosity of the panel as well as to gauge the uniformity of the panel with higher signal strength indicating lower porosity levels. This technique was used by fellow researcher Lance Lowe [17] and is discussed further in Chapter 4 along with the scans from each panel. All scans used in this thesis were conducted by researchers Lance Lowe, Brahmaji Vasantharo, Scott Smith, and Robert Matthews.

3.3.2 Outer Box Pressure Variation

The rst method of porosity introduction attempted was varying the vacuum level on the outer box during the degas phase of the prestaging process. This technique

26 was similar to a single vacuum processing method where the only vacuum applied was to the bag. In this method, the pressure was varied from full vacuum up to no vacuum. Nine panels were made in this way to determine what range of porosity could be achieved with this technique. It was determined that with no outer vacuum during the Degas phase, panels with approximately 3.0% maximum porosity could be created. Panels with vacuums of 23, 20, 17, and 14 in. Hg were produced and compared to panels produced with full vacuums. Table 3.1 Figure 3.8 show the data for panels created with this method. The general trend was higher porosity with lower vacuum level. The average thickness of this panel was 0.042 in. with a standard deviation of 0.00044 in. measured in 24 locations. Table 3.1. Vacuum Pressure Variation Porosity Comparison. Panel # Vacuum Level (in Hg) Void Fraction 21 0 2.87 23 14 1.92 24 14 0.20 25 17 0.52 26 17 0.90 27 20 0.35 28 20 0.40 29 23 0.02 30 23 0.58 17 27 0.04 18 27 0.13

3.3.3 Glass Microballoons

The second method of porosity introduction tried was the inclusion of glass microballoons. These microballoons are used in some marine and aerospace applications as a resin ller to reduce weight. To determine the eect the microballoons

27
Void Fraction vs. Vacuum Level 3

2.5

2 Void Fraction (%)

1.5

0.5

10

15 Vacuum Level (in. Hg)

20

25

30

Figure 3.8. Graph of Void Fraction vs. Vacuum Level on the ply interface, some information about their size distribution was needed. Five small 300 m by 300 m slides of the microballoons were examined in a Scanning Electron Microscope (SEM) by lab technician Wayne Hawkins and were found to have a large size variation. The largest and smallest microballoons were found to be 76.88 m and 3.75 m, respectively with a mean and standard deviation of 27.13 m and 13.34 m, respectively. Figure 3.9 shows a sample of the microballoons. The large sphere in the center was 76.87 m in diameter. In panel 54, a 3-inch wide strip of microballoons was introduced in the three middle ply interfaces during layup (Figure 3.10). The microballoons were applied by hand with a smearing action. The average thickness of this panel was 0.046 in. with a standard deviation of 0.0016 in. measured in 21 locations.

28

Figure 3.9. Sample of microballoons at 800

Figure 3.10. Location of AIBN or Microballoons Insertion During Layup

29

Figure 3.11. Bag Bridging Technique 3.3.4 Bag Bridging

Another idea to create controlled porosity was the use of vacuum bag bridging. In this process, a wooden rod was placed inside the bag, over the laminate to lift the bag o of the laminate directly underneath. Figure 3.11 shows the setup used to create the bridge. The bridge should remove the compacting force of the bag from a portion of the laminate. Dimensional analysis of the panel showed that, the panel was generally thicker underneath the bridge than on the edges. The average thickness of this panel was 0.047 in. with a standard deviation of 0.0060 in. measured in 21 locations. However, in the bridged region the panel measured up to 0.065 in. thick. The thickest part of the panel was in the very center where the pieces for microscopic examination were cut.

30

Figure 3.12. AIBN Chemical Chain [18] 3.3.5 AIBN Foaming Agent

The nal method attempted for introducing porosity was the application of a foaming agent. AIBN is a expanding foam chemical agent often used as a catalyst in many chemical reactions. It is a hydrocarbon chain with nitrogen attached at both ends. As the temperature increases, the hydrocarbon chain begins to break down and release nitrogen gas. Yoshida et al. [11] used a similar agent in their experiment to create trapped air pockets called AZDN. According to Yoshida, 1 gram of AZDN will give o 137 cm3 of nitrogen gas. The AIBN was dissolved in acetone so that it could be sprayed onto the laminae during the lay-up procedure. A model paint sprayer with an aerosol spray can was used to apply the mixture. By doing this, the acetone evaporated quickly leaving behind only the AIBN. The unfortunate problem with this method was the inability to accurately determine the amount of AIBN applied to the laminae since some of the mixture is lost to the surrounding atmosphere. The amount of AIBN applied could not be measured because it was less than 1 gram. This dierence was too small to be measured with any mass balance that was available for this research. The average thickness of this panel was 0.043 in. with a standard deviation of 0.00091 in. measured in 24 locations. Two panels were made with the addition of this mixture

31 while keeping all other parameters constant. Two more panels were made with the added change of removing the outer vacuum during the Degas phase as in the vacuum variation method. It was believed that this combination might create a compounding eect and boost the void content beyond what could be created with one method alone.

CHAPTER 4 POROSITY MEASUREMENT METHODS & RESULTS

The previous chapter focused on the manufacturing methods used to produce the specimens for this research. This chapter will look at porosity measurement. Different methods of calculating porosity will be discussed rst followed by the discussion and results of the porosity measurements made in this research.

4.1 Porosity Measurement Methods

Over the years, many methods have been introduced to determine the relative porosity, or void fraction, of a composite laminate. Each method has its strengths and weaknesses. Methods used for this research will be discussed here along with other methods that were considered but not used.

4.1.1 Density

The porosity measurement method in ASTM standard D2734 [20] uses the density of the resin matrix, ber reinforcement and total composite along with the resin content of the total composite to determine the void fraction. Accurate measurements must be made of the resin density and can be done using ASTM standard D792 or D1505. Any error in this measurement will result in a large error later, perhaps leading to the calculation of a negative void fraction in low porosity specimens. The density of the bers should be measured using ASTM D792. Information from the manufacturer on both resin and ber densities may be used if the results are certied for that batch of material. Resin content should be measured per ASTM 32

33 standard D2584. These results are then inserted into Equation 4.1 to determine the void fraction of the composite

V = 100 Md

g r + dr dg

(4.1)

where:

V = void content, volume %, Md = measured density of specimen, r = resin, weight %, g = ber, weight %, dr = density of resin, and dg = density of ber.

According to Judd [10], the accuracy of this method is 0.50%. This method was not used in this research because of the lack of experience with the procedures and the availability of other better known methods. However, this method would be a good verication of results found with other methods.

4.1.2 Matrix Digestion

Another ASTM standard method to determine void fraction in a composite material is D3171 [21]. In this procedure, piece of the material is placed in a hot acid to dissolve the matrix material. The remaining reinforcement material is dried and weighed to determine the weight of the bers. This method is a destructive test, and

34 can be prohibitive in some situations. Also, some facilities may not be equipped to the handle and store the strong acids and vent the fumes that can be produced during this process. From the weights of the initial sample and the processed bers, along with the densities of the specimen, bers and matrix, the void fraction is calculated from Equation 4.2.

Vv = 100 (Vr + Vm ),

(4.2)

where:

Vv = void volume percent in the specimen, Vr = volume percent of ber in the specimen, Vm = volume percent of resin in the specimen.

The accuracy of this method is not stated in the standard, but only fractional dierences of more than 0.5% are considered in calculations. This would indicate that this method has an accuracy of 0.50% like the previously discussed method. This method was not used in this research because of the hazard associated with the digestion acids.

4.1.3 Ultrasonic C-Scan

Ultrasonics are one of the most useful porosity measurement methods because it is nondestructive. The sample and a transducer are submerged together in water

35 which acts as a coupling agent between the two. A high frequency sound wave is sent through the sample by a pulse receiver transducer and the echo of the signal is picked by the same transducer. As the signal passes through the sample it is scattered or absorbed by irregular features such as porosity and foreign matter inclusions. This reduces the strength of the signal returned to transducer. As the number of these irregular features increase, the overall mean signal returned decreases. The signal amplitude is then plotted as a histogram. From this the mean signal strength is determined which indicates the amount of porosity in the sample. In general, a higher mean signal strength indicates lower porosity. Steiner [19] studied the ability of C-scans to detect dierent types of defects inside composite materials. Porosity was detected in samples with void fractions ranging from 0.17% to 3.57%. The mean signal strength of the histogram of the scan was found to depend greatly on the porosity content. Steiner noted the success of the method at detecting the presence of porosity, but noted that in order to dene the level of the porosity, a number of known porosity level specimens would have to be scanned to build a comparison database. This would also have to be done for each material system examined. C-scanning was also used Grelsson [6] and Kan et al. [7] in their work to study porosity in composites. Another advantage to this method was that the entire specimen is examined. The data gathered from this method produced a full color plot of the entire specimen scanned so that areas of signal strength change can be easily identied. However, as noted by Steiner, this method must be calibrated with standard samples. These samples must be veried by other existing methods and therefore, cannot have an accuracy better than that of the verication method as discussed by Judd [10].

36 The verication of this method for this research was done with the help of Lowe [17]. Several panels were fabricated, scanned, and then examined by light microscopy. The porosity level was then calculated from digital image analysis software. Lowe then compared these measured porosity numbers to the bulk and zoomed C-scan histogram data that was collected to determine a mapping from signal strength to porosity level.

4.1.4 Micrography

Although not an ASTM standard, the microscopic examination method is often used to determine porosity levels. In this method, a small specimen is cut, mounted, ground, polished and then examined with a microscope to quantify porosity levels. In early studies, a point counting method was used where a very ne grid was placed over the specimen and the void fraction calculated by counting the grid intersections that coincided with a void and dividing by the total number of points in the grid. Working with the point counting technique, Judd et al. [10] proposed that accuracy for this method is about 0.50% and is as accurate as other current techniques such as matrix digestion and density measurement. In recent years, advances in computer hardware and software have produced a number of graphics analysis programs that will count dened particles in a digital image. This method can be adapted to measure porosity if there is sucient contrast between the voids and the surrounding material. Cilley et al. [22] found that this method could be used in conjunction with other techniques and provide acceptable results. There are two major drawbacks to this method. First, like matrix digestion, microscopic examination is a destructive measure. This is prohibitive in a production environment where the area of interest cannot be cut and still be used. Second, it is

37 an area measurement not a volumetric measurement which reduces its validity. To increase condence in this method, multiple sections can be examined from dierent areas. Micrography can also be used in conjunction with another method to increase condence in measurements. Micrography was used in this research along with ultrasonic C-scan to obtain all porosity measurements. This combination was chosen because both methods are fairly easy to conduct and prevalent in industry. Also, the two methods work well together to verify each other. In this research, panels were scanned after fabrication to determine the uniformity of the panel and to look for any unusual features such as inclusions, delaminations, or larger concentrated areas of porosity. The scan could then be used to decide where to cut the specimens for micrographic examination. The porosity value from this specimen could then be compared to the mean signal strength for the entire panel as well as for the small region it came from. This process is called zooming, where the histogram from a small region of interest was examined to determine the local mean signal strength and therefore the porosity in that region. This process was also used by Lowe [17] in his research to calibrate the C-scanning technique.

4.2 Porosity Measurement Results

4.2.1 Specimen Preparation

After fabrication, the panels were sectioned for microscopic examination and porosity measurement. The panels were cut on a tile saw with an aluminum oxide abrasive cuto wheel to produce a specimen approximately one inch wide. This process produced a good edge with the individual laminae visible to the unaided

38 eye. These sectioned pieces were then mounted in a two-part castable epoxy, or cold mount, and allowed to cure overnight. Grinding and polishing was done with a Buehler automated grinder-polisher. ASM Handbook 9 [23] was consulted to determine the proper method for surface preparation. The grinding was done with 320, 400, and 600 grit grinding discs while ushing with water. Polishing was done with 6 m and 3 m diamond suspension and 1 m cerium oxide on soft matte pads. The specimens were ground and polished in 30 second intervals and examined for adequate material removal, then repeated as necessary.

4.2.2 Digital Imaging

The specimens were photographed with a digital microscopy system and analyzed with the computer software program Image-Pro Plus [24]. The photographs are taken through an inverted light microscope at approximately 140 magnication. Eight photographs were taken from each specimen, which were then examined individually to determine their void fraction. The void fraction was determined by the program using the built in particle counting function. The program dierentiated between the voids which appear black from the matrix and bers which appear gray and white. There was some level of subjectivity involved in determining the contrast level to be considered a void. This could be overcome by the experience gained from repeated measurements and familiarity with the process and the material. The average particle size, number of particles and void fraction for each image was calculated by the program. The void fraction was then calculated as the particle area divided by the total specimen area. The average void fraction of the eight images was taken to

39 get the void content for the total specimen. Four specimens from dierent locations out of each panel were examined to increase the validity of the measurement. This method was veried by the manual point counting method described by Judd [10]. The comparison was done on one sample in work done by Hoy et al. [26] using a computer program called Global Lab [25]. A verication study was done to determine if suciently accurate results could be obtained using the Image Pro Plus software. One sample was examined using both programs by the same user. Measurements of 2.57% and 2.86% were obtained for the chosen test piece with the two dierent programs. This dierence is well within the accepted 0.5% accuracy of the method.

4.2.3 Image Analysis

The porosity measurements from Image-Pro Plus are listed in Table 4.1. The measured void fraction of the chosen standard panel was actually the largest of any standard panel created in this research. It is likely that some features counted as porosity were really not porosity. The vacuum pressure variation panel had a lower measured void fraction than expected and did not appear to be very dierent from the control panel. However, examination in the ESEM shows that these panels are actually quite dierent in their porosity content. Panels 54 and 61 have high measured porosity contents as expected. Panel 57 was expected to have a high measured porosity content but apparently does not. The nature of the porosity, or lack thereof, is of great interest and is examined later in this chapter. In Figures 4.1 to 4.5 the third and fth layers are oriented parallel to the cut. This made measuring porosity in these areas dicult if not impossible. These layers have many dark regions where bers are dropping in and out of the plane that appear

40 Table 4.1. Porosity Measurement Results. # Method Void Fraction (%) Mean Signal Strength Standard 0.75 49.39 Pressure Variation 1.05 17.00 Microballoons 2.01 38.87 Bag Bridging 0.36 40.89 AIBN 5.93 8.10 Higher mean signal strength indicates lower porosity.

Panel 35 51 54 57 61 Note:

to be porosity to the software. Other features like scratches from metallographic preparation can also get counted as porosity. This all contributes to the 0.5% accuracy that is cited by Judd [10]. The standard panel specimens from panel 35 had a void fraction of 0.75%. However, further examination of the photomicrographs shows that the actual value is much less than that which was evident from the C-scan data. In Figure 4.1, the cross section of a standard panel is shown. Notice that there were no voids visible anywhere on the cross-section. Further, the individual laminae were touching each other and are dicult to distinguish in some places. There were also no noticeable resin rich regions. All of these factors dene a good quality standard panel with low porosity. The vacuum pressure variation specimen from panel 51 had a void fraction of 1.05%. In Figure 4.2, notice the dark spots that were visible in the middle region of the specimen. These were voids in the laminate. They were primarily located at the laminae interfaces and were generally elliptical in shape and sometimes group together to form larger voids. There were very few resin rich regions visible in this specimen. Panel 54 contained microballoons and, as expected, had a higher void fraction of 2.01%. However, the porosity created in this panel was unlike the porosity created

41

Figure 4.1. Inverted Light Microscope Photomicrograph of Panel 35

Figure 4.2. Inverted Light Microscope Photomicrograph of Panel 51

42

Figure 4.3. Inverted Light Microscope Photomicrograph of Panel 54 in panel 51 with the vacuum pressure variation. In Figure 4.3, the cross-section of a specimen from panel 54 is shown. The dark spherical objects were the microballoons that were included in the layup between the plys. Also, the microballoons were still located at the laminae interfaces and did not migrate through the layers. Their presence also created large resin layers at each interface where they were present. The presence of this large deposit of resin was of great concern, because it changes the way the laminate behaves, likely reducing the interlaminar shear strength. Panel 57 was the bridged sample. This specimen was expected to have a very high void fraction, but when measured, was found to have a very small void fraction at 0.36%. Surprisingly, this measurement was less that the standard panel. However, notice in Figure 4.4 the angled layers in the the top of the laminate. In this gure, the specimen was getting thicker on the right side by approximately 0.015 in. This phenomena was curious since the specimen was believed to have been cut directly

43

Figure 4.4. Inverted Light Microscope Photomicrograph of Panel 57 through the bridged region. Very little porosity was visible, but other problems exist that were not yet evident and will be seen in the Section [?]. Panel 61 was sprayed with the AIBN foaming agent and was also expected to have a high void fraction. The measured porosity was 5.93%, the highest of any panel manufactured in this research. A typical cross section is shown in Figure 4.5. The poor quality of this specimen was immediately evident. Large voids along with signicant pockets of resin were visible throughout the specimen. In earlier specimens with the other methods, voids were only found at the laminae interfaces. Here, they were found in all locations through the panel and not just along the three middle interfaces where the AIBN was sprayed. This spread indicates that the nitrogen gases from the AIBN did migrate during the cure cycle.

44

Figure 4.5. Inverted Light Microscope Photomicrograph of Panel 61 4.2.4 Comparison with C-scan Data

Figure 4.6 shows the C-scan of panel 35. In this gure, small blue lines were noticed in the midst of the green surrounding areas that indicated a drop in signal strength. The green indicated a higher mean signal strength while the blue represented a lower mean signal strength. The blue lines were caused by the impressions left by the wrinkled non-porous plys during curing and were visible on the surface of the panel. The red spots at the top were most likely caused by an air bubble trapped underneath the panel in the water tank. This scan also indicated that this panel was fairly uniform. From Table 4.1, the mean signal strength was 49.39, the highest of any of the ve panels used in this study which would indicate that the porosity possibly lower than the 0.75% measured by micrography.

45

Figure 4.6. Mean Signal Strength Ultrasonic C-Scan of Panel 35 Figure 4.7 shows the C-scan of panel 51. A distinct dierence could be seen between this panel and panel 35 in Figure 4.6. The darker colors show a drop in mean signal strength and indicated an increase in porosity. This was consistent with the higher void fraction measured by micrography of 1.05%. Also note that this panel also appeared to be fairly uniform indicating that the porosity was evenly distributed. Table 3.1 from Chapter 3 is repeated in Table 4.2 with the mean signal strengths included for comparison. When the mean signal strength of panel 51 was compared to those done in earlier work, it appeared that panel 51 was more porous than the 1.05% measured by micrography. Figure 4.8 shows the ultrasonic C-scan of panel 54. From this scan, it was easy to see that the microballoons were applied in a vertical band in the center. This darker blue signal indicated a lower mean signal strength and more porosity than the surrounding area. The lighter blue areas on the left and right indicated a much lower

46

Figure 4.7. Mean Signal Strength Ultrasonic C-Scan of Panel 51 Table 4.2. Vacuum Pressure Variation Porosity Comparison. # Outer Vacuum (in Hg) % Porosity C-Scan Mean Signal Strength 27 0.04 59.11 27 0.13 57.49 0 2.87 32.79 14 1.92 28.34 14 0.20 29.15 17 0.52 33.20 17 0.90 39.27 20 0.35 45.34 20 0.40 49.80 23 0.02 55.87 23 0.58 42.11

Panel 17 18 21 23 24 25 26 27 28 29 30

porosity region than the center but perhaps more than in panel 35. This observation indirectly veried the void fraction of 2.01% measured by micrography.

47

Figure 4.8. Mean Signal Strength Ultrasonic C-Scan of Panel 54 The C-scan of panel 57 is shown in Figure 4.9. As with the microballoons, the area where the bridge was applied is easily seen from the C-scan. A rst look at the Cscan would imply that there was a large region of porosity under the bridge. However, the unevenness indicated that any created porosity was not as evenly distributed as with the microballoons or the vacuum pressure variation. The panel also had thickness variations of up to 40% in this middle region. Since the time of ight of the sound wave was used to calculate the mean signal strength, this thickness change may be the reason behind the mean signal strength change. This observation is supported by the void fraction of 0.35% measured by micrography. However, it was later discovered that the panel was manufactured incorrectly, with the bridged region running parallel to the outer layer bers instead of perpendicular. The rst clue was that the low signal region in Figure 4.9 was perpendicular to those in the microballoon panel and the AIBN panel. At rst, this was thought

48

Figure 4.9. Mean Signal Strength Ultrasonic C-Scan of Panel 57 to be a mistake made when the panel was scanned. The second clue was that if the micrography specimen was cut through the bridged region, the thickness should not change. However, Figure 4.4 clearly shows that the specimen thickness is changing. These observations were veried by measuring the strip that the specimen was cut from. One unfortunate result is that the tensile test specimens cut later to miss the bridged region entirely. Panel 55 was made with a 4 in. wide band of AIBN sprayed on each interface and other parameters left constant. The overall mean signal was 41.30, which would indicate only a small rise in porosity because the baseline from Panel 35, which was 49.39 from Table 4.1. However, the C-scan of panel 55 shown in Figure 4.10 shows that there was very little mean signal signal drop in the region where the mixture was sprayed.

49

Figure 4.10. Mean Signal Strength Ultrasonic C-Scan of Panel 55 This small signal drop indicated that the nitrogen gas escaped out of the laminate, or it was spread evenly throughout the laminate. Because it was unlikely that the latter happened, so it was concluded that the nitrogen gas was escaping. It was possible that this might happen if the AIBN was breaking down during the Degas phase of the cycle and was being completely evacuated from the laminate along with entrapped air and devolved gases. Material data sheets obtained from DuPont [18] conrm this suspicion with an equation. The half life of the molecule at a given temperature is computed from Equation 4.3,

log (t1/2 ) = 7142(1/T ) 18.355,

(4.3)

50 where:

t1/2 = half life in minutes, T = temperature in Kelvin.

At the 225 F prestaging temperature, the half life of the AIBN is only 2.75 minutes. Since it took the laminate 52 minutes to heat up to this point from room temperature and then dwelled there for 25 minutes, it seems very likely that the nitrogen gas was escaping from the laminate during the prestage phase. Therefore, panel 61 was made the same way as panel 55 except the outer vacuum was left o during the degas phase to attempt to capture the nitrogen within the layers. Also, only the middle three interfaces were sprayed with AIBN in panel 61. The C-scan of panel 61 can be seen in Figure 4.11. In this gure the area where the AIBN was applied can be clearly distinguished from the surrounding area implying that the nitrogen gas was entrapped in this region and producing signicant porosity. This conclusion was supported by the 5.93% void content measured by micrography.

4.2.5 SEM Examination

One specimen from each panel was further prepared for examination in the Scanning Electron Microscope (SEM). The specimens were coated with a thin layer of gold to discharge electrons in the chamber since the specimens are nonconductive. The purpose of examining in the SEM was to determine the shape and size of the porosity produced and to determine the eect the dierent methods might have on

51

Figure 4.11. Mean Signal Strength Ultrasonic C-Scan of Panel 61 the laminae interfaces. (Please refer back to Section 3.3 for an explanation of the specimen numbering scheme.) Specimen 35-5-1 from the standard panel 35 was examined to determine a baseline for comparison with other specimens. An example of a void-free laminae interface is shown in Figure 4.12. This gure shows how the laminae interfaces should look in a panel with no unusual processing parameters or introduced foreign matter. There is no resin layer between laminae and there is no porosity on the cross section. Even with a ner magnication (Figure 4.13) there is no discernible resin layer between plys. Specimen 51-6-1 from panel 51 was examined to determine the eect of vacuum pressure variation. Figure 4.14 shows a view of the typical cross section. From this view, the panel appears to be of fairly good quality with no large defects of discontinuities present. Figure 4.15 shows a closer view of the middle interfaces.

52

Figure 4.12. SEM Photomicrograph of Panel 35 Laminae Interfaces

Figure 4.13. SEM Photomicrograph of Panel 35 Close-up of Laminae Interfaces

53

Figure 4.14. Photomicrograph of Panel 51 Laminae Interfaces Notice that the porosity in this panel was located predominately at the laminae interfaces and furthermore, mainly at the laminate centerline. It is not certain if the location of these sites was a property of the method used or a function of the amount of porosity present. All panels manufactured by this method exhibited a similar pattern. Specimen 54-5-2 was examined to further determine how the microballoons aected the laminate. From Figure 4.16, the microballoons can be seen to be widely distributed along the middle three interfaces. In the SEM, they glow white because the electrons build up on the sharp edges, causing them to charge. A closer look in Figure 4.17 shows that there are many more microballoons present than were visible in lower magnication pictures. Some broken pieces that have been lled with resin are clearly visible and may likely create a structural weakness in the panel. Also, the resin rich laminae interface region is the same thickness as the microballoons,

54

Figure 4.15. Photomicrograph of Panel 51 Close-up of Laminae Interfaces indicating that the bers are being pushed apart by the microballoons. This will certainly reduce the interlaminar shear strength and result in a panel that has a dierent mechanical behavior than the standard panel. Specimen 57-5-1 from the bridged specimen shows why this method as implemented is unacceptable. In Figure 4.18, the laminate was getting thicker and some of the resin that was dispersed throughout the laminate was visible. In Figure 4.19, the resin pockets were clearly seen. This feature accounted for the increase in specimen thickness that was measured earlier and was seen in the photomicrographs. However, there was little or no porosity in this specimen as indicated from the micrography measurements. This lack of porosity was of little consequence compared to the drastic changes in resin content and thickness seen here. Specimen 61-5-2 shows more porosity and resin pockets than any other panel. The edges of the voids appear white because of electron charging. Figure 4.20 shows

55

Figure 4.16. Photomicrograph of Panel 54 Laminae Interfaces

Figure 4.17. Photomicrograph of Panel 54 Close-up of Laminae Interfaces

56

Figure 4.18. Photomicrograph of Panel 57 Laminae Interfaces

Figure 4.19. Photomicrograph of Panel 57 Close-up of Laminae Interfaces

57

Figure 4.20. Photomicrograph of Panel 61 Laminae Interfaces much of what was seen earlier from the photomicrographs from the light microscope (Figure 4.5. Figure 4.21 shows a close-up of the cross-section. Here the extent of the porosity can really be seen. Laminae are almost destroyed in some places by resin layers and voids. Laminae thickness also vary greatly from point to point. Laminae interfaces were also not consistently lined up along the length as seen in panel 35. The voids have permeated every layer of the material. This was denitely a high porosity, low quality specimen.

4.2.6 Pore Characterization and Measurement in SEM

The pictures taken in the SEM were then measured using built-in functions of the software. Pictures from each specimen were examined to determine the changes in specimen thickness and ply thickness as well as to measure the size of resin rich regions

58

Figure 4.21. Photomicrograph of Panel 61 Close-up of Laminae Interfaces and individual pores. Laminate and laminae thickness variations will be discussed rst, followed by pore classication and measurement. Table 4.3 shows the average thickness of the two middle plys for the ve laminates. There was a noticeable thickness increase in the microballoons and bridged specimens when compared to the standard panel. The variation also increased greatly in the bridged and AIBN panels. Examples of measurements from each panel are shown in Figures 4.22 through 4.35. Table 4.3. Specimen Thickness Variation of Middle Two Laminae. Panel # Method Mean Thickness (m) Std. Dev. (m) 35 Standard 274.9 11.8 51 Pressure Variation 254.6 5.5 54 Microballoons 375.8 4.6 57 Bag Bridging 317.1 34.2 61 AIBN 254.7 21.9

59

Figure 4.22. Panel 35 Thickness Variation Measurement of Middle Two Laminae

Figure 4.23. Panel 51 Thickness Variation Measurement of Middle Two Laminae

60

Figure 4.24. Panel 54 Thickness Variation Measurement of Middle Two Laminae

Figure 4.25. Panel 57 Thickness Variation Measurement of Middle Two Laminae

61

Figure 4.26. Panel 61 Thickness Variation Measurement of Middle Two Laminae The dierent types of voids were examined next by the same method. The voids present were divided into three types according to shape according to the ratio of major to minor axis: linear over 5:1, round up to 2:1, elliptic 2:1 to about 5:1. No voids were found in panels 35 and 57 as was discussed earlier. The voids in panel 54 were created completely by the presence of the microballoons and their size and variation was discussed Section 3.3.3 so they will not be discussed here. In panel 51, the voids were generally round with a few ellipses. In some cases, the voids coalesced into larger linear voids that resemble delaminations. Figures 4.27, 4.28, and 4.29 show round, elliptic and linear voids from panel 51.

62

Figure 4.27. Representative Round Void in Panel 51

Figure 4.28. Representative Elliptic Void in Panel 51

63

Figure 4.29. Representative Linear Void in Panel 51 In panel 61, there were many more of each type of void. Many small round voids were found throughout with a few ellipses. In the plys where the bers were parallel to the cut surface, there were many linear voids that extend for as much as 1 mm. Figures 4.30, 4.31, and 4.32 show a round, elliptic and linear void from panel 61. In addition to porous regions, resin rich regions were another area of concern. Panel 35 had no noticeable resin rich regions. Panel 54 had numerous resin rich regions created at the laminae interfaces and were discussed in Section 4.2.5. Panel 51 had some such regions and one of these is shown in Figure 4.33.

64

Figure 4.30. Representative Round Void in Panel 61

Figure 4.31. Representative Elliptic Void in Panel 61

65

Figure 4.32. Representative Linear Void in Panel 61

Figure 4.33. Representative Resin Rich Region in Panel 51

66

Figure 4.34. Representative Resin Rich Region in Panel 57

Figure 4.35. Representative Resin Rich Region in Panel 61

CHAPTER 5 MATERIAL TESTING METHODS & RESULTS

The previous chapter looked at the porosity measurement techniques and results. This chapter will discuss the mechanical testing performed on the test specimens. Tensile testing, damage threshold testing and fatigue testing are all discussed in this chapter.

5.1 Equipment Description

A MTS 810 servohydraulic test frame with a 20000 pounds maximum load cell was used to perform tensile and fatigue testing in this research. The frame was equipped with MTS 647 hydraulic wedge grips with interchangeable grip faces to grip at or round samples. The system was run by a MTS TestStar IIs controller. The extensometer used for tensile testing was a MTS model 632.25B-20 which has a gage length of 2 in. The load frame and setup used are shown in Figure 5.1. Tensile and fatigue specimens were prepared per ASTM Standard D5687 [27]. The panels were cut with an abrasive cuto wheel with water coolant. This method was compared to a ban saw and was found to produce a cleaner edge. The specimens were tabbed with E-glass berglass tabs to improve gripping and reduce damage done to the specimen by the grips. The tabs were bonded with 3M AF167 Structural Weld which cures at 250 F for 90 minutes. A tabbed specimen is shown in Figure 5.2. No tab bevel angle was used and was the only noted exception to the ASTM standard. However, according to Adams et al. [28] there is widening acceptance that a nonbeveled edge, or bevel angle of 90 F, is a usable geometry and has even been adopted

67

68

Figure 5.1. MTS Test Frame with Specimen and Extensometer

Figure 5.2. Composite Specimen with E-Glass Tabs by the International Organization for Standardization (ISO) as their standard test conguration.

5.2 Material Characterization

The material system chosen for this study is widely used in research and industry. As a result, the material properties of the system are fairly easy to nd in

69 the public domain. One resource used for this research was the website of The University of California, San Diegos Composites and Aerospace Structures Laboratory [14]. This site contained a complete set of material properties for IM-6/3501-6 with a ber volume of 63.5%. However, it was desired to verify these properties before using them in any further research since dierent processing techniques were used. Two unidirectional 8-ply laminates and one [45]8S laminate were made to verify some of the material properties. The two unidirectional panels were cut so that one had transverse outer layer bers and the other longitudinal outer layer bers. The other panel was cut so that the top layer was oriented at +45 . A three element 45 rosette strain gage was applied to one specimen of each lot for tensile testing. The results of this verication study are shown in Table 5.1. The values for E11 ,E22 , 12 , and 23 were in close agreement with those obtained from the UCSD website. A value for G12 could not be obtained because the equipment needed to make the measurement was not available. Table 5.1. Summary of Material Characterization Property Measured UCSD [14] 6 E11 22.15 10 psi 23.30 106 psi E22 1.187 106 psi 1.395 106 psi 12 0.285 0.2965 23 0.285 0.2965 G12 not measured 0.9161 106 psi

5.3 Tensile Testing

Samples from each panel were prepared for testing according to ASTM D3039 [29]. Each specimen was measured for thickness and width variation before testing.

70 Some specimens were out of specication on the width tolerance, 1% of the width, when measured over the entire specimen length. These specimens were then remeasured in the gage section to see if that region of the specimen was acceptable and if so, the specimens were used. The only other discrepancy between the tests performed and the ASTM standard was the use of a 90 bevel angle on the tabs. A summary of the tensile tests is presented in Table 5.2. The data for the standard panel indicated an ultimate stress of about 95000 psi with an ultimate strain of 0.011 . Panel 51 had only slightly lower values for each, indicating that its monotonic behavior was very similar to a standard panel. Panel 54 had a much lower ultimate stress of 84000 psi , but a similar ultimate strain. This lower strength value seems to conrm the suspicion that the large resin rich regions at the ply interfaces is adversely aecting the materials behavior. Panel 57 had a similar ultimate stress and strain to the standard panel but with increased scatter in the stress data. The bridge was arranged such that these specimens were not cut through the bridge and were therefore identical to those from panel 35. The mistake was discovered during the later stages of this research after all samples had been used. Panel 61 behaved similar to panel 54, exhibiting greatly reduced ultimate stress and strain values.

5.4 Damage Threshold Test

Five samples were tted with two longitudinal strain gauges each in an attempt to measure the damage threshold of the material. The specimens were loaded to a specic strain level, scanned, and loaded to a higher strain. This process was repeated for strain levels of 2500 , 5000 , 7500 , and 10000 with the exception that no scan was taken after 10000 . The purpose of this test was to determine what threshold strain level would cause damage in the specimen as any weakness imparted

Panel 35 51 54 57 61

Table 5.2. Summary of Tensile Test Results. Ultimate Strength (psi) Ultimate Strain ( ) Ultimate Load (lbs) Measured Std. Dev Measured Std. Dev Measured Std. Dev 95675 6574 0.01115 0.00089 4139 275 94942 2828 0.01063 0.00169 3793 100 84187 3964 0.01092 0.00067 4294 208 95413 14569 0.01194 0.00047 4711 229 82778 7040 0.00924 0.00174 3684 284

71

72 by the porosity introduction would be evident in this test. In each test, the specimen was aligned in the machine the same way so that gage 1 was on the back side and gage 2 was on the front. This was done so that any bending eects would not be missed since because of normal dierences between the two gage readings. A nal strain load of 12000 was to be applied after the previous scan. However, the rst two specimens tested broke before reaching this strain level. It was decided to proceed with each specimen to failure and record the nal strain reading. The results of this test are shown in Table 5.3. No apparent pattern could be seen in the data. It would perhaps have been more benecial to perform this test in specimens with a notch or central hole so that the porosity was in the vicinity of a stress concentration. This scenario might give a better indication as to the aw sensitivity of the material. Table 5.4 shows the C-scan results for these specimens after the rst three strain levels. In most cases, the initial mean signal strength was lower than that measured after the rst strain level. It is unknown why this occurred. However, after the rst level, the trend was as expected, decreasing signal strength with increasing damage. Figures 5.3 through 5.12 show the C-scans before any testing and after 7500 for each specimen. In each sample, the strain gauge and lead wires were visible in the second picture.

Table 5.3. Damage Threshold Test Results 2500 5000 7500 Sample Gage 1 Gage 2 Load Gage 1 Gage 2 Load Gage 1 Gage 2 Load 35-7 2488 2612 779 4860 5036 1525 7366 7538 2304 51-10 2545 2485 832 5002 5070 1672 7575 7650 2516 54-9 2515 2472 882 5050 5044 1796 7540 7077 2688 57-9 2478 2510 895 5100 5072 1840 7545 7563 2747 61-9 2500 2450 855 5040 4945 1724 7555 7460 2583 Note: All loads measured in pounds. Note: * Denotes audible damage during loading.

Gage 1 10011 10068 10119 10068 10166

10000 Gage 2 10160 10160 10060 10021 10077

Load 3041 3264 3541* 3587* 3459

73

74

Table 5.4. C-Scan Results from Damage Threshold Test Mean Signal Strength at Strain Increment Sample 0 2500 5000 7500 35-7 28.34 34.41 34.82 33.60 51-10 18.22 15.79 17.81 14.98 54-9 29.55 36.44 39.27 33.60 57-9 37.25 36.89 38.46 32.39 61-9 6.48 6.48 5.67 4.86

Figure 5.3. Preliminary C-scan of Strip 35-07

Figure 5.4. Final C-scan of Strip 35-07

75

Figure 5.5. Preliminary C-scan of Strip 51-10

Figure 5.6. Final C-scan of Strip 51-10

Figure 5.7. Preliminary C-scan of Strip 54-09

76

Figure 5.8. Final C-scan of Strip 54-09

Figure 5.9. Preliminary C-scan of Strip 57-09

Figure 5.10. Final C-scan of Strip 57-09

77

Figure 5.11. Preliminary C-scan of Strip 61-09

Figure 5.12. Final C-scan of Strip 61-09

78 5.5 Fatigue Testing

Specimens were also fabricated for fatigue testing and were tested per ASTM D3479 [30]. The only exceptions to this standard were the same as those noted for ASTM D3039. The tests were conducted in load control with a sine wave at 10 Hz. A thermocouple was attached to a setup piece and cycled to determine if any heating eects were present during loading. A temperature increase of 12 F was noted during one million cycles and was determined to be acceptable. Panels 36 and 37 were selected from the remaining standard panels for the fatigue tests. Five samples from panel 36 were tested per ASTM D3039 to determine the average ultimate strength and thereby establish the load levels for fatigue testing. There were not enough specimens to test the recommended six at each load level. Load levels were chosen for the remaining fteen specimens to ll in the part of the stress-life curve of interest. To establish the approximate stress-life curve, the rst four specimens were tested at four dierent load levels to see what lives would be expected. These tests were run on four specimens remaining from panel 36. The nal specimen from panel 36 and the ten specimens from panel 37 were then divided between the established ranges. Before cycling, the specimens were examined with C-scans and vibrational tests to get a baseline for the specimen with no damage. These specimens were then run in blocks, or fractions, of the expected life. After each block, C-scans were taken to determine the damage accumulated during the cycling. Vibrational tests were done to detect any changes in natural frequency. Examination of the specimens was planned to be done four or ve times during the process to track damage accumulation. However, the specimens from panel 37 began failing sooner

79
Fatigue Life, R=0.1 1 Panel 36 Panel 37 0.95

0.9

0.85 Percent Failure Stress

0.8

0.75

0.7

0.65

0.6

0.55

0.5 2 10

10

10 Cycles to Failure (Log (N))

10

10

Figure 5.13. Panels 36 and 37 Fatigue Plot, ult =10600 psi. than expected and only one or two examinations were made. The results of the fatigue tests are listed in Table 5.5. To determine why specimens from panel 37 behaved this way, the data for all fatigue tests was plotted in Figure 5.13 with the vertical axis being the percentage of the failure stress of 106000 psi. When the data was plotted as two dierent sets from the two panels, it was clearly seen that the two panels follow two dierent stress life curves. This implied some dierence in the behavior of the two panels. The manufacturing parameters were identical between the two so some other dierence may be present. At rst, it was thought that there might be some aect from submerging the specimens underwater for the ten minutes needed to take the C-scan. A similar sample was weighed and submerged for forty minutes and weighed every ten minutes. During this time, there was no increase in total specimen mass, indicating no water absorption.

Table 5.5. Fatigue Test Results. Sample # % Failure Load Stress Level (psi) # Cycles Notes 36-6 0.9 95727 404 no delam. 36-7 0.8 85090 2308 signicant delam., some long. splitting 36-8 0.7 74454 58906 signicant delam., some long. splitting 36-9 0.6 63818 1000000 * extreme delam., some long. splitting 36-10 0.8 85090 1288 some delam. 37-1 0.75 85090 1438 little delam. 37-2 0.75 85090 97 bad test run, failed by buckling 37-3 0.7 74454 7224 some delam. 37-4 0.7 74454 8344 some delam. 37-5 0.7 74454 7631 some delam. 37-6 0.75 63818 2559 some delam. 37-7 0.65 63818 16795 some delam. 37-8 0.65 63818 20527 signicant delam. 37-9 0.6 53182 78773 extreme delam., signicant long. splitting 37-10 0.6 53182 65370 extreme delam., signicant long. splitting Note: Average Failure Stress 106000 psi (From specimens 35-1,2,3,4,5) Note: Load Ratio R = 0.1 Note: * Denotes test run out.

80

81 One possibility for this discrepancy in fatigue life was misalignment during laminae lay-up and cutting. An existing ANSYS nite element model was modied to include misaligned plys to determine what the stress and strain increase would be in this case. The model was created to measure strain levels at three gage locations on the surface: the load direction (Gage 1), perpendicular to the load direction (Gage 3) and halfway in between (Gage 2). The bers in the load direction and the +45 plys were increased by 7.5 to simulate misalignment. This 7.5 would account for an average of 3.75 misalignment from both operations. The data from the model is listed in Table 5.6. This data indicate a 16.8% increase in strain and a 12% increase in stress in the load direction. While a signicant increase, this would not be enough to cause the extreme dierences in stress life that was noticed in the fatigue specimens. Table 5.6. Changes in Stress and Strain from Fiber Misalignment Oset of 0 Plys Oset of +45 Plys Gage 1 Gage 2 Gage 3 0 0 2177 641 -682 7.5 0 2299 445 -753 7.5 7.5 2544 841 -699

Another idea was to examine the cut edge of a specimen that had not been tested. Perhaps there was some signicant damage induced during the cutting operation. Figure 5.14 shows a stereo microscope image of a cut edge. There was no noticeable damage from the saw that would contribute to the premature failure of any of the specimens. The edges of the broken specimens were also photographed and examined to see if there was any information about the failure there. While there was an abundance of information about the failures on the edges, there were no clues as to what might have made them fail prematurely. There was signicant delamination in all specimens

82

Figure 5.14. Saw Cut Edge of Composite Specimen that ran for more than 10,000 cycles which may indicate that the interlaminar shear stresses were very high. An edge of one of the failed specimens is shown in Figure 5.15. Notice that the individual laminae have separated completely and that there are many areas where the laminae have cracks running across their thickness. Also in Figure 5.15, there were regions where the laminae appear to have buckled. This was observed in many samples that were run at higher load levels. It is probably due to an actual compressive stroke by the machine in the last cycles of the specimen as failure had already begun to occur. The machines response may not have been quick enough to keep up with the rapidly changing compliance of the specimen so as it tried to compensate, it increased the stroke and placed the specimen in compression. Readings on the load meter after failure read as low as 1000 pounds in compression. This had no eect on the actual life of the specimen since it occurred after failure had already begun.

83

Figure 5.15. Failed Edge of Specimen 37-7

CHAPTER 6 CONCLUSIONS & RECOMMENDATIONS

The previous chapters dealt with the procedures and tests conducted to produce the data for this research as well as the analysis of that data. This chapter will focus on the conclusions drawn from that data and make recommendations for future work based on those conclusions.

6.1 Summary & Conclusions

Microscopic examination as well as ultrasonic C-scan data from all four porosity methods were taken and compared to the same data for a standard panel. Mechanical testing was done to determine any eects the methods might have on the mechanical properties of the laminate. After reviewing this data, the four porosity introduction methods were ranked in the following manner: 1. vacuum pressure variation 2. chemical foaming agent introduction 3. microballoon introduction 4. bag bridging (should retry). The vacuum pressure variation technique was found to work well when porosity levels between 0.0% and 3% were desired. The photomicrographs and tensile test results indicated that this method did not signicantly alter the laminate behavior. This method was also the only one to produce naturally occurring porosity. Another benet of this method was the ability to accurately dene the processing parameters by varying the vacuum level in discrete increments. In terms of real production parts, this 0.0% to 3% is very realistic. 84

85 The addition of the AIBN foaming agent was found to be desirable only when porosity levels above 3% were desired. The changes made to the laminae and their interfaces made them less like the naturally occurring porosity seen in Section 2.1 than the previous method. The inability to measure the amount of agent applied to the laminate will make it dicult to reliably produce a given porosity level with any accuracy. The addition of glass microballoons does not appear to be a reasonable way to introduce porosity. The changes in the laminae interfaces were too dierent from naturally occurring porosity. Production hardware with this type of porosity would probably never be usable. The large resin-rich regions that are created at the laminae interfaces should reduce the interlaminar shear strength as it did the tensile strength and should be veried in future research. Although the porosity created with this method did not resemble naturally occurring porosity, microballoons could be used to produce NDE standard specimens for training. The vacuum bag bridging technique does not appear to be a good option in the manner attempted. The tensile test results gave no insight into the eect the increased resin content had on the laminate since this region was missed due to mistakes made in manufacturing. However, the photomicrographs contained enough information to suggest that the method was not successful as-implemented since there was no porosity created in the specimen examined,. This fact alone rules out this method as it was implemented. However, future work might nd a better way of producing the desired eect with this idea.

86 6.2 Recommendations For Future Work

The rst recommendation from this research is that more testing is needed to determine an accurate method for producing porosity. A procedure could be developed for the vacuum pressure variation technique to produce samples at 0.5% void fraction increments from 0.0% to 3%. This would require producing panels at very ne increments of pressure change and characterizing them with the methods used in Chapter 4 of this research. Also, the vacuum bag bridging technique should be attempted again with a dierent setup. It is possible that some other conguration could create controlled porosity, since it is believed that this is one way that porosity occurs naturally in production. Perhaps bridging on a more localized level might produce acceptable results. Other porosity measurement techniques could also be tried to verify current results. The ASTM standard density and matrix digestion tests oer an good opportunity to verify measurements taken with micrography and further test the ultrasonic C-scan method. Infrared thermography is another method that has been suggested for use in this eld. Next, interlaminar shear stress tests should also be conducted on all of the porosity introduction techniques to further determine the eects of the methods on the mechanical properties. The Isoipescu shear test method (ASTM D5379) or the Two-Rail shear test method (ASTM D4255) are the most likely tests to be used. In another test, multiple samples should be produced from one method with dierent void fractions for fatigue testing. This type of testing could help characterize the long term eects of porosity on the fatigue life of composites. Within this testing, multiple geometries should be examined including straight sections, open holes, and

87 notched specimens. This data would give more insight into the behavior of porosity in the presence of a stress concentration. Such information could lead to the disposition of as-built hardware with naturally occurring porosity. Two more areas that should be examined are curved members and residual stresses. Since composite members are frequently used as T-shaped or L-shaped brackets or stieners, the behavior of these geometries in the presence of porosity is of interest. Residual stress eects in these curved members would be another area of interest for future work. Current work by Venkatesan [31] has investigated this behavior for standard specimens. Adding the presence of porosity and curvature to this type of research would be of interest to the manufacturing and design communities. Finally, tensile and fatigue tests should be conducted in the presence of porosity after low velocity impact. This has applications in the area of service induced damage where an event such as a tool strike during service may induce signicant damage to a composite structure that is not visible. Currently, this type of damage structure may be replaced or reworked when much less work may required to keep the structure in service.

REFERENCES

88

89 [1] Strong, A. B. Fundamentals of Composites Manufacturing: Materials,Methods, and Applications. Dearborn: Society of Manufacturing Engineers, 1989. [2] Jones, R. M. Mechanics of Composite Materials, Second Edition. Philadelphia: Taylor & Francis, Inc., 1999. [3] Walker, J., Telephone conversation and emails, October 15, 2003 to November 5, 2003. [4] Gay, D., Hoa, S. V., and Tsai, S. W., Composite Materials, Design and Applications. Boca Raton: CRC Press, 2003. [5] Garrett, R. A., Eects of Manufacturing Defects and Service-Induced Damage on the Strength of Aircraft composite Structures, Composite Materials: Testing and Design, ASTM STP 893, pp. 5-33, 1986. [6] Grelsson, B., Correlations Between Porosity Content, Strength and Ultrasonic Attenuation in Carbon Fibre Laminates, Materials & Design, Vol. 13, no. 5, pp .275-278, 1992. [7] Kan, Han-Pin, Bhatia, Narain M., and Mahler, Mary A., Eect of Porosity on Flange-Web Corner Strength, Composite Materials: Fatigue and Fracture, ASTM STP 1110, pp. 126-139, 1991. [8] Pipes, R. B., Interlaminar Shear Fatigue Characteristics of Fiber-Reinforced Composite Materials, Composite Materials: Testing and Design, ASTM STP 546, pp. 419-432, 1974. [9] Hancox, N. L., The Eects of Flaws and Voids on the Shear Properties of CFRP, Journal of Materials Science, Vol. 12, pp. 884-892, 1977. [10] Judd, N. C. W., Wright, W. W., Voids and Their Eects on the Mechanical Properties of Composites - An Appraisal, SAMPE Journal, January/February, pp. 10-14, 1978. [11] Yoshida, H., Ogasa, T., and Hayashi, R. Statistical Approach to the Relationship Between ILSS and Void Content of CFRP, Composites Science and Technology Vol. 25, pp. 3-18, 1986.

90 [12] Dharan, C. K. H., Fatigue Failure Mechanisms in a Unidirectionally Reinforced Composite Material, Fatigue of composite Materials, ASTM STP 569, pp. 171188, 1975. [13] Dill, C. W., Tipton, S. M., Glaessgen, E. H., and Branscum, K. D., Fatigue Strength Reduction Imposed by Porosity in a Fiberglass Composite, Damage Detection in Composite Materials, ASTM STP 1128, pp. 152-162, 1992. [14] University of California San Diego, available from http://casl.ucsd.edu/, accessed on June 24, 2002. [15] Sherwin, G. R. Non-autoclave Processing of Advanced Composite Repairs, Adhesion & Adhesives Vol. 19, pp. 155-159, 1999. [16] Omega CN4620 Temperature Controller, Users Guide CN4420, CN4520, CN4620 & CN4720 Series Temperature / Process Controllers. Omega, 2002. [17] Lowe, D. L., Porosity Determination in Thin Graphite-Epoxy Composite Laminates Using Histograms of C-Scans, A Thesis Presented for the Master of Science Degree in Mechanical Engineering, Tennessee Technological University, Cookeville, Aug. 2003. [18] DuPont, available from http://www.dupont.com/vazo, accessed October 31, 2002. [19] Steiner, K. V., Defect Classication in Composites Using Ultrasonic Nondestructive Evaluation Techniques, Damage Detection in Composite Materials, ASTM STP 1128, pp. 72-84, 1992. [20] American Society of Materials Testing, D 2734 - 94 - Standard Test Method for Void Content of Reinforced Plastics, 2001 Annual Book of ASTM Standards, Vol. 8.02, pp. 106-108, 2001. [21] American Society of Materials Testing, D 3171 - 99 - Standard Test Method for Constituent Content of Composite Materials, 2001 Annual Book of ASTM Standards, Vol. 15.03, pp. 118-126, 2001. [22] Cilley, E., Roylance, D., and Schneider, N., Methods of Fiber and Void Measurement in Graphite/Epoxy Composites, Composite Materials: Testing and Design, ASTM STP 546, pp. 237-249, 1974.

91 [23] American Society of Metals, Fiber Composite Materials, ASM Handbook, Vol 9 Metallography and Microstructures, pp. 587-597. [24] Image-Pro Plus Version 4.5, Image-Pro Plus Reference Guide for Windows. Media Cybernetics, 2001. [25] Global Lab Image Version 2.00, Image Processing and Analysis Software for Microsoft Windows, Data Translation, 1992. [26] Wilson, C. D., Hoy, D. E. P., Understanding the Service Life of Composites, NCAM Project 58404, July. 2002. [27] American Society of Materials Testing, D 5687/D 5687 M - 95 - Standard Guide for Preparation of Flat Composite Panels with Processing Guidelines for Specimen Preparation, 2001 Annual Book of ASTM Standards, Vol. 15.03, pp. 302-317, 2001. [28] Adams, D. F., Carlsson L. A., Pipes R. B., Experimental Characterization of Advanced Composite Materials, Third Edition. Boca Raton: CRC Press, 2003. [29] American Society of Materials Testing, D 3039/D 3039 M - 00 - Standard Test Method for Tensile Properties of Polymer Matrix Composite Materials, 2001 Annual Book of ASTM Standards, Vol. 15.03, pp. 106-117, 2001. [30] American Society of Materials Testing, D 3479/D 3479 M - 96 - Standard Test Method for Tension-Tension Fatigue of Polymer Matrix Composite Materials, 2001 Annual Book of ASTM Standards, Vol. 15.03, pp. 146-151, 2001. [31] Venkatesan, K, Hole-drilling Finite Element Method for Determination of Residual Stresses in Graphite-Epoxy Composite Laminates, A Thesis Presented for the Master of Science Degree in Mechanical Engineering, Tennessee Technological University, Cookeville, December 2003.

APPENDIX

92

APPENDIX A : TENSILE TEST DATA PLOTS

93

94

12

x 10

Stress vs Strain for Specimen 351

10

Stress (psi)

0.002

0.004

0.006 0.008 Strain (in/in)

0.01

0.012

0.014

Figure A.1. Tensile Plot for Specimen 35-1

12

x 10

Stress vs Strain for Specimen 352

10

Stress (psi)

0.002

0.004

0.006 0.008 Strain (in/in)

0.01

0.012

0.014

Figure A.2. Tensile Plot for Specimen 35-2

95

12

x 10

Stress vs Strain for Specimen 353

10

Stress (psi)

0.002

0.004

0.006 0.008 Strain (in/in)

0.01

0.012

0.014

Figure A.3. Tensile Plot for Specimen 35-3

12

x 10

Stress vs Strain for Specimen 354

10

Stress (psi)

0.002

0.004

0.006 0.008 Strain (in/in)

0.01

0.012

0.014

Figure A.4. Tensile Plot for Specimen 35-4

96

12

x 10

Stress vs Strain for Specimen 511

10

Stress (psi)

0.002

0.004

0.006 0.008 Strain (in/in)

0.01

0.012

0.014

Figure A.5. Tensile Plot for Specimen 51-1

12

x 10

Stress vs Strain for Specimen 512

10

Stress (psi)

0.002

0.004

0.006 0.008 Strain (in/in)

0.01

0.012

0.014

Figure A.6. Tensile Plot for Specimen 51-2

97

12

x 10

Stress vs Strain for Specimen 513

10

Stress (psi)

0.002

0.004

0.006 0.008 Strain (in/in)

0.01

0.012

0.014

Figure A.7. Tensile Plot for Specimen 51-3

12

x 10

Stress vs Strain for Specimen 514

10

Stress (psi)

0.002

0.004

0.006 0.008 Strain (in/in)

0.01

0.012

0.014

Figure A.8. Tensile Plot for Specimen 51-4

98

12

x 10

Stress vs Strain for Specimen 541

10

Stress (psi)

0.002

0.004

0.006 0.008 Strain (in/in)

0.01

0.012

0.014

Figure A.9. Tensile Plot for Specimen 54-1

12

x 10

Stress vs Strain for Specimen 542

10

Stress (psi)

0.002

0.004

0.006 0.008 Strain (in/in)

0.01

0.012

0.014

Figure A.10. Tensile Plot for Specimen 54-2

99

12

x 10

Stress vs Strain for Specimen 543

10

Stress (psi)

0.002

0.004

0.006 0.008 Strain (in/in)

0.01

0.012

0.014

Figure A.11. Tensile Plot for Specimen 54-3

12

x 10

Stress vs Strain for Specimen 544

10

Stress (psi)

0.002

0.004

0.006 0.008 Strain (in/in)

0.01

0.012

0.014

Figure A.12. Tensile Plot for Specimen 54-4

100

12

x 10

Stress vs Strain for Specimen 571

10

Stress (psi)

0.002

0.004

0.006 0.008 Strain (in/in)

0.01

0.012

0.014

Figure A.13. Tensile Plot for Specimen 57-1

12

x 10

Stress vs Strain for Specimen 572

10

Stress (psi)

0.002

0.004

0.006 0.008 Strain (in/in)

0.01

0.012

0.014

Figure A.14. Tensile Plot for Specimen 57-2

101

12

x 10

Stress vs Strain for Specimen 573

10

Stress (psi)

0.002

0.004

0.006 0.008 Strain (in/in)

0.01

0.012

0.014

Figure A.15. Tensile Plot for Specimen 57-3

12

x 10

Stress vs Strain for Specimen 574

10

Stress (psi)

0.002

0.004

0.006 0.008 Strain (in/in)

0.01

0.012

0.014

Figure A.16. Tensile Plot for Specimen 57-4

102

12

x 10

Stress vs Strain for Specimen 611

10

Stress (psi)

0.002

0.004

0.006 0.008 Strain (in/in)

0.01

0.012

0.014

Figure A.17. Tensile Plot for Specimen 61-1

12

x 10

Stress vs Strain for Specimen 612

10

Stress (psi)

0.002

0.004

0.006 0.008 Strain (in/in)

0.01

0.012

0.014

Figure A.18. Tensile Plot for Specimen 61-2

103

12

x 10

Stress vs Strain for Specimen 613

10

Stress (psi)

0.002

0.004

0.006 0.008 Strain (in/in)

0.01

0.012

0.014

Figure A.19. Tensile Plot for Specimen 61-3

12

x 10

Stress vs Strain for Specimen 614

10

Stress (psi)

0.002

0.004

0.006 0.008 Strain (in/in)

0.01

0.012

0.014

Figure A.20. Tensile Plot for Specimen 61-4

APPENDIX B: LIST OF PHOTOGRAPHS INCLUDED ON CD

104

105 The material for this section is still being compiled and will be included in the nal copy. REG 11/14/03.

VITA

Richard Eugene Gregory was born on December 12, 1975, in Parsons, TN. He attended Riverside High School where he graduated valedictorian in May of 1994. He was a member of the Boys Scouts of America Troop 29 for 7 years where he earned the rank of Eagle Scout. He attended Middle Tennessee State University for three years before transferring to Tennessee Technological University to complete his Bachelors Degree in Mechanical Engineering. On June 26, 1999, he married Kathryn McDowell in Lebanon, TN. Upon graduation, he worked for TRW, Inc. in Rogersville, TN for two years before returning to TTU to pursue his Masters Degree.

106