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Adhesive Bonding Technology and Testing
Adhesive Bonding Technology and Testing

Ricardo João Camilo Carbas


Eduardo André Sousa Marques
Alireza Akhavan-Safar
Ana Sofia Queirós Ferreira Barbosa
Lucas Filipe Martins da Silva
Authors All books published by WILEY-VCH are carefully
produced. Nevertheless, authors, editors, and
Dr. Ricardo João Camilo Carbas publisher do not warrant the information
INEGI - Inst. of Science and Innovation contained in these books, including this book,
in Mechanical Engineering to be free of errors. Readers are advised to keep
Dept. of Mechanical Engineering in mind that statements, data, illustrations,
Rua Dr. Roberto Frias s/n procedural details or other items may
4200-465 Porto inadvertently be inaccurate.
Portugal
Library of Congress Card No.: applied for
Dr. Eduardo André Sousa Marques
INEGI - Inst. of Science and Innovation British Library Cataloguing-in-Publication Data
in Mechanical Engineering A catalogue record for this book is available
Rua Dr. Roberto Frias 400 from the British Library.
4200-465 Porto
Portugal Bibliographic information published by
the Deutsche Nationalbibliothek
Dr. Alireza Akhavan-Safar The Deutsche Nationalbibliothek lists
INEGI - Inst. of Science and Innovation this publication in the Deutsche
in Mechanical Engineering Nationalbibliografie; detailed bibliographic
Rua Dr. Roberto Frias 400 data are available on the Internet at
4200-465 Porto <http://dnb.d-nb.de>.
Portugal
© 2023 WILEY-VCH GmbH, Boschstraße 12,
Dr. Ana Sofia Queirós Ferreira Barbosa 69469 Weinheim, Germany
INEGI - Inst. of Science and Innovation
in Mechanical Engineering All rights reserved (including those of
Rua Dr. Roberto Frias 400 translation into other languages). No part of
4200-465 Porto this book may be reproduced in any form – by
Portugal photoprinting, microfilm, or any other
means – nor transmitted or translated into a
Prof. Lucas Filipe Martins da Silva machine language without written permission
University of Porto from the publishers. Registered names,
Dept. of Mechanical Engineering trademarks, etc. used in this book, even when
Rua Dr. Roberto Frias s/n not specifically marked as such, are not to be
4200-465 Porto considered unprotected by law.
Portugal
Print ISBN: 978-3-527-35051-3
Cover Image: © Jenson/Shutterstock ePDF ISBN: 978-3-527-83800-4
ePub ISBN: 978-3-527-83801-1
oBook ISBN: 978-3-527-83802-8

Typesetting Straive, Chennai, India


v

Contents

Preface xi

1 Simple Practical Demonstrations 1


1.1 Importance of Loading Mode on Bonded Joint Performance 1
1.1.1 Introduction 1
1.1.2 Equipment 1
1.1.3 Materials 2
1.1.4 Safety Precautions 2
1.1.5 Experimental Procedure 2
1.1.5.1 In Class 2
1.1.5.2 In the Laboratory 3
1.2 Surface Treatments and Methods to Evaluate Surface Energy 6
1.2.1 Introduction 6
1.2.2 Equipment 7
1.2.3 Materials 8
1.2.4 Safety Precautions 8
1.2.5 Experimental Procedure 8
1.2.5.1 In Class 8
1.2.5.2 In Laboratory 9
1.3 Stress Distribution Along the Overlap Length 12
1.3.1 Introduction 12
1.3.2 Equipment 13
1.3.3 Materials 13
1.3.4 Safety Precautions 13
1.3.5 Test Procedure 13
1.4 Visual Identification of Defects in Adhesive Joints 15
1.4.1 Introduction 15
1.4.2 Equipment 17
1.4.3 Materials 17
1.4.4 Safety Precautions 17
1.4.5 Test Procedure 17
1.5 Failure Analysis of Adhesive Joints 19
1.5.1 Introduction 19
vi Contents

1.5.2 Equipment 20
1.5.3 Materials 20
1.5.4 Safety Precautions 20
1.5.5 Test Procedure 21

2 Production and Testing 25


2.1 Bulk Specimens 25
2.1.1 Introduction 25
2.1.2 Adhesive Pouring Technique 25
2.1.3 Metallic Mold 26
2.1.4 Adhesive Application 30
2.1.5 Curing Procedure 31
2.1.6 Machining Procedure 33
2.1.7 Testing Procedure 35
2.2 Thick Adherend Shear Specimens 35
2.2.1 Introduction 35
2.2.2 Metallic Mold 36
2.2.3 Surface Treatment of Adherends 37
2.2.4 Geometrical Control Using Shims 40
2.2.5 Specimen Manufacture 41
2.2.6 Final Specimen Preparation 42
2.2.7 Testing Procedure 42
2.3 Fracture Mechanics Specimens 44
2.3.1 Introduction 44
2.3.2 Metallic Mold 48
2.3.3 Surface Treatment of Adherends 49
2.3.4 Adhesive Spacers 50
2.3.5 Specimen Manufacture 50
2.3.6 Final Preparation of Specimens 51
2.3.7 Testing Procedure 52
2.3.8 Data Reduction Schemes 53
2.4 Single-Lap Joint Specimens 56
2.4.1 Introduction 56
2.4.2 Surface Treatment of Adherends 56
2.4.3 Joint Manufacture 57
2.4.4 Final Preparation of Specimens 60
2.4.5 Testing Procedure 60

3 Laboratorial Activities and Report Examples 65


3.1 Effect of Surface Treatment on the Mechanical Behavior of Adhesively
Bonded Joints 65
3.1.1 Introduction 65
3.1.1.1 Joint Strength Prediction 66
3.1.2 Work Description 67
3.1.3 Materials 67
Contents vii

3.1.3.1 Adherends (Tables 3.1 and 3.2) 67


3.1.3.2 Adhesive (Table 3.3) 67
3.1.4 Experimental Work 67
3.1.5 Report 68
3.1.5.1 Introduction 68
3.1.5.2 Experimental Procedure 71
3.1.5.3 Materials 71
3.1.5.4 Failure Load Prediction 72
3.1.5.5 Experimental Results and Discussion 72
3.1.5.6 Conclusions 78
3.2 Effect of Adhesive Type and Overlap Length on the Failure Load of
Adhesively Bonded Joints 79
3.2.1 Introduction 79
3.2.2 Work Description 83
3.2.3 Materials 83
3.2.3.1 Adherends 83
3.2.3.2 Adhesives (Table 3.7) 84
3.2.4 Experimental Work 84
3.2.5 Report 84
3.2.5.1 Introduction 84
3.2.5.2 Materials 86
3.2.5.3 Prediction of the Failure Loads 86
3.2.5.4 Experimental Results 90
3.2.5.5 Discussion 94
3.2.5.6 Conclusions 97
3.3 Effect of Adhesive Thickness on the Failure Load of Adhesively Bonded
Joints 97
3.3.1 Introduction 97
3.3.2 Work Description 98
3.3.3 Materials 99
3.3.3.1 Adherends: 99
3.3.3.2 Adhesives: 99
3.3.4 Experimental Work 99
3.3.5 Report 99
3.3.5.1 Introduction 100
3.3.5.2 Experimental Details 100
3.3.5.3 Prediction 101
3.3.5.4 Experimental Results 102
3.3.5.5 Failure Surfaces 103
3.3.5.6 Conclusion 103
3.4 Effect of Overlap Length on the Strength and Failure Mechanism of
Composite Adhesive Joints 104
3.4.1 Introduction 104
3.4.2 Work Description 105
3.4.3 Materials 105
viii Contents

3.4.3.1 Adherends: 105


3.4.3.2 Adhesives (Table 3.17) 105
3.4.4 Experimental Work 105
3.4.5 Report 106
3.4.5.1 Introduction 106
3.4.5.2 Characterization of the Tested Joints 107
3.4.5.3 Theoretical Prediction of Failure Load 112
3.4.5.4 Comparison with Experimental Results 115
3.4.5.5 Conclusions 116
3.5 Modeling a Single-Lap Joint Using Finite Element Analysis and
Cohesive Zone Modeling 117
3.5.1 Introduction 117
3.5.2 Work Description 117
3.5.3 Materials 117
3.5.3.1 Adherends: 117
3.5.3.2 Adhesives (Table 3.25) 118
3.5.4 Modeling Procedure 118
3.5.5 Report 118
3.5.5.1 Introduction 118
3.5.5.2 Module/Part 122
3.5.5.3 Module/Property 124
3.5.5.4 Module/Section 128
3.5.5.5 Module/Step (First Phase) 129
3.5.5.6 Module/Load 131
3.5.5.7 Module/Mesh 132
3.5.5.8 Module/Step (Second Phase) 134
3.5.5.9 Module/Job 136
3.5.5.10 Module/Visualization 137
3.6 Case Study in Joint Design for a Structural Automotive Application 139
3.6.1 Introduction 139
3.6.2 Report 139
3.6.2.1 Introduction 140
3.6.2.2 Design Brief 140
3.6.2.3 Adhesive Selection 142
3.6.2.4 Surface Treatment Selection 145
3.6.2.5 Material Properties 146
3.6.2.6 Joint Design 148
3.6.2.7 Numerical Models 152
3.6.2.8 Design Validation 156
3.6.2.9 Design for Manufacturing 160
3.6.2.10 Quality Control Techniques 162
3.6.2.11 Health and Safety Concerns 163
References 163
Contents ix

4 Essay and Multi-choice Questions 165


4.1 Essay Questions 165
4.2 Multi-choice Questions 166

Solutions 187
Essay Questions – Example Answers 187
Multi-choice Questions – Solutions 190

Index 191
xi

Preface

This book is intended to serve as a didactic tool to support both those teaching and
learning the subject of adhesive bonding. While the companion book “Introduction
to Adhesive Bonding” is mostly dedicated to the theoretical aspects of this joining
technology, this book is more concise and highly focused on hands-on learning, with
exercises and their solutions and multiple experimental activities.
The book is divided into four parts. The first is dedicated to simple practical
demonstrations of adhesive bonding. These are all simple activities suitable to be
carried out in a classroom setting, which quickly highlight the advantages and
limitations of this technique. The second part is dedicated to production and testing
of specimens that are used to characterize adhesives and the most commonly used
types of joints. The third part describes in detail multiple laboratorial activities
suitable for implementation in the laboratorial classes of engineering courses. These
activities explore aspects such as the manufacture of defect-free bonded joints,
the effects of geometry and materials properties in adhesive joint testing, surface
preparation and joint design and strength prediction, among many others. Lastly,
a set of exercises is provided in the form of developmental questions and multiple
choice questions. This last part focuses on all of the knowledge areas discussed in
the companion “Introduction to Adhesive Bonding” book. All problems are provided
with solutions, and many are fully solved, helping bachelor or masters students in
their study and providing evaluation reference materials for teachers.
The authors would like to thank Paulo Nunes for the help in the preparation of
figures.
They also want to thank the team of WILEY, especially Felix Bloeck, for the excel-
lent cooperation during the preparation of this book.

Porto, Portugal, 2022 Ricardo João Camilo Carbas


Eduardo André Sousa Marques
Alireza Akhavan-Safar
Ana Sofia Queirós Ferreira Barbosa
Lucas Filipe Martins da Silva
1

Simple Practical Demonstrations

1.1 Importance of Loading Mode on Bonded Joint


Performance
1.1.1 Introduction
Adhesive bonding shows many advantages over more traditional methods of joining
such as bolting, brazing, and welding or even the use of mechanical fasteners. No
other joining technique is so versatile, and its transversality lies in its capacity to join
different materials, its ability to ensure permanent assembly, and its ease of use. In
fact, a well-designed bonded joint allows for a reduction in production costs, while
maintaining proper mechanical properties of the joint.
Adhesives work by exploring the adhesion phenomena, and they are usually
polymeric materials, typically thermosetting, that, compared to materials that are
joined in structural applications (such as metals and composites), show a much
lower strength. Nonetheless, adhesive joints can be applied to a wide diversity of
structures, withstanding different types of loads. To understand the mechanics of a
bonded joint, it is important to first establish that the behavior of the joint is highly
dependent on the type of loads it is sustaining. In an attempt to obtain the highest
joint strength, it is fundamental to load the adhesive under forces acting in the
plane of the adhesive layer, minimizing peeling loads. Joints are generally more
resistant when shear-stressed because the adhesive layer is relatively well aligned
with the loading direction. In these conditions, the entirety of the adhesive layer
can positively contribute to sustain the load (see Figure 1.1). Joints subjected to
cleavage or peel stresses are much weaker than those subjected to shear because the
stresses are concentrated in a very small area. All the stress is located at the edge of
the joint (see Figure 1.1).

1.1.2 Equipment
● One set of scissors
● Tensile testing machine

Adhesive Bonding Technology and Testing, First Edition. Ricardo João Camilo Carbas,
Eduardo André Sousa Marques, Alireza Akhavan-Safar,
Ana Sofia Queirós Ferreira Barbosa, and Lucas Filipe Martins da Silva.
© 2023 WILEY-VCH GmbH. Published 2023 by WILEY-VCH GmbH.
2 1 Simple Practical Demonstrations

F
Shear Cleavage
F

Figure 1.1 Schematic representation of the shear and cleavage loads acting on adhesive
joints.

1.1.3 Materials
● One roll of double-sided foam adhesive tape
● Small aluminum beams

1.1.4 Safety Precautions


Apply the necessary safety procedures for operating a test machine.

1.1.5 Experimental Procedure


1.1.5.1 In Class
Peel the adhesive tape off the roll by applying a pulling force or “peeling” action as
shown in Figure 1.2. See how easily it peels away, even if the adhesive is quite strong.

Figure 1.2 Adhesive joint under


pull-out force.

Adhesive
tape roll
1.1 Importance of Loading Mode on Bonded Joint Performance 3

Adhesive

Adhesive

F
F

Figure 1.3 Adhesive joint subjected to shear stress, with the area being overlapped with
and without the adhesive.

Now, cut two strips of adhesive tape, approximately 10 cm long. Bond the two
strips parallel to each other with an overlap of approximately 3 cm. Bond the glued
side of one strip to the unglued side of the other strip (see Figure 1.3). Pull on the
joint in order to try to separate the strips by loading them parallelly to the adhe-
sive layer, thereby subjecting the adhesive to shear, as schematically represented in
Figure 1.3. It will be much harder to separate the joint as we are now loading it in
shear; however, because of the low stiffness of the tape, it will bend and introduce
some peeling loads, as shown in Figure 1.3, and this peeling can promote debonding.
Repeat the same procedure, but this time, join the strips so that the sides that have
adhesive are in direct contact, as represented in Figure 1.4. When the joint is made
between the glued side of both strips, it is impossible to separate the strips under
shear. Ultimately, the strips will break, while the bonded area remains intact.

1.1.5.2 In the Laboratory


In order to better understand the influence of load type when an adhesive joint is
used, the same tape will be bonded to an aluminum plate, and the response for
two different types of load (shear and peel) will be studied using a universal tensile
machine.
4 1 Simple Practical Demonstrations

Adhesive

Adhesive

F F

Figure 1.4 Adhesive joint subjected to shear stress, with the area being overlapped with
the adhesive on both strips.

To this aim, the same tape will now be applied to metal (aluminum) adherends.
Cut an adhesive tape strip, approximately 10 cm long, and join it to the surface of an
aluminum adherend with a 3 cm overlap. This adhesive joint is subjected to shear
stress, as shown in Figure 1.5. As the adherend is much stiffer, this adhesive joint is
now subjected to an almost uniform shear stress.
The procedure will now be replicated, but this time, the forces exerted will be in a
peeling direction. Therefore, it is recommended for the tape strip to be slightly longer
so that it can be easily pulled off. Cut an adhesive tape strip, approximately 15 cm
long, and join it to the surface of an aluminum adherend with 3 cm of overlap. This
adhesive joint can now be subjected to peeling stress, as shown in Figure 1.6.
A comparison of the loads applied on the manufactured joints can be done man-
ually or using a testing machine. Manually, it is possible to “feel” that the forces
are different, but they cannot be quantified. Therefore, using a universal testing
machine, the behavior of the joints loading under different types of stresses and dif-
ferent surface states can be easily quantified, leading to different results. Figure 1.7
shows a schematic representation of the peel and shear forces. As “felt” in a man-
ual test, when an adhesive joint is tested in peel stress, at first, it is necessary to
exert a greater force to peel off the adhesive, but over the course of the test, the force
required decreases and the joint eventually fails. In turn, when the adhesive joint is
being tested at shear, the force required gradually increases until failure occurs.
1.1 Importance of Loading Mode on Bonded Joint Performance 5

Aluminum

Adhesive

Figure 1.5 Adhesive joint using adhesive tape and aluminum adherends, subjected to
shear stresses.

Aluminum

Adhesive

Figure 1.6 Experimental testing procedure of an adhesive joint using adhesive tape and
aluminum adherends, subjected to shear stresses.
6 1 Simple Practical Demonstrations

Figure 1.7 Schematic


Load representation of the shear
and peel behavior of an
Shear load adhesive joint.

Peel load

Displacement

1.2 Surface Treatments and Methods to Evaluate


Surface Energy
1.2.1 Introduction
Surface preparation of an adherend is key to achieve a strong and durable adhesive
joint, and it is a process step that should never be taken lightly. The type and
the quality of surface preparation will unequivocally determine the behavior of
the joint. Surface treatments can be divided into two major groups: passive and
active treatments. Briefly, we can explain this categorization by saying that passive
treatments do not change the chemical nature of the material surface and the active
processes chemically change the adherend by cleaning and removing weak layers
on the surface.
How a liquid will wet a surface will mainly dictate the level of adhesion between
the adhesive and the adherend. The formation of a drop of liquid on a solid surface
is described by the contact angle, 𝜃, between the solid surface and the tangent to the
surface of the liquid at the point of contact as schematically presented in Figure 1.8.
The aim of surface treatments is to obtain a clean and wettable surface. Unfortu-
nately, there is no standardized procedure or equipment to assess surface cleanliness.
Furthermore, a clean surface is difficult to define and sometimes even quantify. One
way of evaluating the level of cleanliness is to say that a surface is clean when no dirt
is visible to the naked eye. However, this is a very subjective process, and the quality
of the surface treatment should always be subject to a strict control.
The value of 𝜃 can vary from zero – when there is complete liquid spreading, and
we are experiencing perfect wetting – to 180∘ when the liquid assumes the shape of
a spherical drop and does not wet the solid at all, as shown in Figure 1.9.

Vapor Figure 1.8 Angle of


contact (𝜃) formed between
θ an adherend surface and a
liquid.
Liquid

Solid
1.2 Surface Treatments and Methods to Evaluate Surface Energy 7

θ 0° 90° 180°
cosθ 1 0 –1

Spread Full Partial γSL = γSV Negligible Non-


wetting wetting wetness wetting

Figure 1.9 Variation of the contact angle of a drop of liquid as a function of its spreading
on a surface.

Water forms spherical drops Water forms a uniform film

Figure 1.10 Wetting of a surface with a liquid before and after surface treatment: (a)
untreated surface and (b) treated surface.

These differences can be easily observed in Figure 1.10, where the same liquid
and the same surface (in this case, a composite material) behave in different ways.
Before the surface treatment, the liquid does not wet the surface, forming very visible
and spherical drops. On the other hand, after surface treatment, it is observed that
the liquid wets the surface, forming a film. The contact angle decreases with the
application of a surface treatment.
In an ideal surface preparation, the contact angle should be as close as possible to
zero to ensure good adhesion. There is a wide range of surface treatments available
for use with adhesive bonding processes, and consequently, the quality of the surface
may vary and lead to different morphologies and surface conditions. However, the
final result of a surface treatment should always be the same: an increase in joint
strength and durability, achieved by promoting adhesion between the materials to
be bonded and the adhesive. Regardless of the procedure used, this should always
be the final goal of the surface treatment.

1.2.2 Equipment
● Plasma generator device
● Pipette
● Dyne pens
8 1 Simple Practical Demonstrations

1.2.3 Materials
● Aluminum adherend (non-degreased surface)
● Aluminum adherend (surface degreased with acetone)
● Polymeric adherend (surface degreased with acetone)
● Polymeric adherend (treated with plasma)
● Water
● Acetone
● Cleaning paper (take care, as chosen paper must not contaminate the surface, not
shred after the addition of the solvent, nor leave residues on the treated surface)

1.2.4 Safety Precautions


Avoid direct contact of acetone with the skin.
The plasma and anodizing treatments should be performed under an effective
air extraction system because harmful volatiles can be released during the process
treatment.
Surface blasting processes must be carried out in accordance with the manufac-
turer’s safety recommendations and PPE must be provided.

1.2.5 Experimental Procedure


Surface treatment can be carried out using both passive and active methods. Depend-
ing on the class of material to be treated, a selection of the best suited methodology
must be performed.

1.2.5.1 In Class
In this demonstration, a passive surface treatment method will be first used (clean-
ing with a solvent, acetone). This process aims to remove oily or greasy areas, which
are the sources of very low wetting and adhesion. In many non-structural bonding
applications, these processes are often sufficient, but they are frequently the first step
of a more complex surface treatment process in structural applications.
Degreasing is the simplest method suitable to obtain a clean surface, decrease the
contact angle, and increase the adhesive spreading. This procedure can be applied
to a wide range of materials, such as polymers, composites, and metals. There are
several methods that can be followed for the application of a solvent. In this demon-
stration, manual cleaning was chosen, as shown in Figure 1.11. Cleaning should
always be carried out in the same direction in order to remove the dirt without
re-contaminating the surface.
An active treatment procedure, as explained, will chemically alter the treated sur-
face. It must therefore be carefully selected, taking into account the material to be
treated.
There are several approaches suitable for measuring the wettability, contact angle,
and consequently the surface energy of a surface. Some are simple techniques, such
as observing the shape of a drop of water, while others are much more complex,
such as measuring the contact angle with specialized goniometers. The use of Dyne
1.2 Surface Treatments and Methods to Evaluate Surface Energy 9

Acetone

Cleaning direction

Cloth

Figure 1.11 Manual cleaning of a surface using acetone and a cloth.

pens is a widely used technique for assessing the quality of surface energy. This
technique is a simple, cheap, and quick method, where pens are used to draw a
line of a special ink along the surface of the adherent and thus visually observe the
behavior of the liquid.
To observe the shape of the drop on the treated surface, it is recommended to
use a liquid whose properties are well known, and for this, distilled water is recom-
mended. Using a pipette, a small drop is placed on the different prepared surfaces.
The analysis of the drop shape will be mainly visual. If the drop has a spherical shape,
this means that the liquid is not properly wetting the surface. If, on the other hand,
the liquid easily spreads on the surface, this means that the treatment is facilitating
the wetting of the liquid on the treated surface. It is easy to see that different surface
preparations lead to different droplet shapes (Figure 1.12).
Dyne pens can also be used to quantify the quality of the surface preparation.
This analysis is more rigorous than the previously described one as the use of these
pens allows us to determine an approximate value of the surface energy. Dyne pens
use calibrated liquids, so if the applied liquid completely wets the surface, we can
then have an approximate idea of a minimum surface energy value. This test is also
very effective in predicting whether the surface shows differences before and after
a surface treatment. Figure 1.13 shows the application of the same calibrated liquid
before and after cleaning with acetone. Before cleaning, the liquid is unable to wet
the surface. After cleaning with acetone, which is a simple and non-invasive surface
preparation, the calibrated liquid can already wet the surface.

1.2.5.2 In Laboratory
A plasma generator will be used to treat the surfaces of polymeric adherends. Plasma
treatment is the most effective technique to increase the surface energy of polymers
because it is responsible for changing the chemistry of polymeric surfaces to be
treated (see Figure 1.14).
10 1 Simple Practical Demonstrations

Without surface preparation With surface preparation

(a) (b)

Figure 1.12 Observation of the shape of a drop of water with a liquid of known properties
on metallic surface without (a) and with (b) surface treatment.

Without surface preparation Cleaned with acetone Figure 1.13 Use of Dyne pens on a
metallic surface before (a) and after
(b) surface preparation.

(a) (b)

Please note that these surfaces should not be touched with hands, avoiding the
introduction of grease that can contaminate the already treated surfaces. It is advis-
able to join the treated surfaces immediately after treatment. If this is not possi-
ble, they should be conveniently stored in a manner that ensures that there is no
contamination.
1.2 Surface Treatments and Methods to Evaluate Surface Energy 11

Figure 1.14 Surface of the polymeric


material to be treated with plasma.

(a) (b)

Figure 1.15 Observation of the shape of a drop of water with a liquid of known properties
on a polymeric surface without (a) and with (b) surface treatment.

Figure 1.15 clearly shows that the wettability is higher when the polymer is
exposed to plasma treatment, and this allows us to conclude that the adhesion is
higher when the polymeric adherends are treated with plasma.
The use of Dyne pens allows us to determine the surface energy of polymeric
materials; this is achieved using different pens with different calibrated liquid ener-
gies, starting with 30 up to 38 mJ/m2 . Figure 1.16 shows that the surface energy of
untreated polymeric adherends is between 30 and 32 mJ/m2 because it is clear that
the liquids of this pens are able to uniformly wet the polymer.
Figure 1.16 shows that the surface energy of the polymeric adherend after treat-
ment with plasma increases from 30 mJ/m2 to more than 38 mJ/m2 . This means
that the surfaces treated will show good adhesion with the adhesive, and after being
bonded, the failure is probably cohesive.
12 1 Simple Practical Demonstrations

(a) (b)

Figure 1.16 Dyne pen application on a polymeric non-treated (a) and plasma-treated (b)
adherend.

1.3 Stress Distribution Along the Overlap Length


1.3.1 Introduction
Tensile loads on a single overlap joint subject the adhesive to shear and peel stresses,
as shown in Figure 1.17. The shear and peel distributions in the adhesive along the
overlap length exhibit a large stress gradient at the end of the overlap, where a stress
concentration is present.
When considering the loads that an adhesive joint can be subjected to, shear
is by far the more preferable for adhesive joints (see Figure 1.18). In this loading
condition, the adhesive layer is relatively well aligned with the load direction,
which means that the entire adhesive layer can contribute positively to support the
load. When designing an adhesive joint, one should always try to ensure that the
adherends carry the load in a manner that is as parallel to the adhesive layer as
possible.
Several analytical models allow the calculation of these stress distributions, as
do many numerical methods such as the use of finite element modeling, which
allows us to obtain precise stress and strain distributions along the adhesive layer,
providing clear information about how loaded a portion of adhesive is under ser-
vice. With this demonstration, it is intended to experimentally show how the strain

Shear Peel

Figure 1.17 Schematic representation of adhesive joints subjected to shear and peel
stresses.
1.3 Stress Distribution Along the Overlap Length 13

Figure 1.18 Typical F


bonded joint geometries for
a joint under shear stress. b F

t
l

τav

τ (shear stress on the adhesive)

(and hence stress) distributions vary along the adhesive layer using a joint where the
adherends are composed of hard rubber and the adhesive is simulated by a relatively
soft foam rubber.

1.3.2 Equipment
● One tensile testing machine
● Black marker pen

1.3.3 Materials
● Two sheets of a hard natural rubber 25 cm × 2.5 cm × 1 cm
● One piece of foam rubber 2.5 cm × 2.5 cm
● Contact adhesive
● Acetone

1.3.4 Safety Precautions


Avoid contact with the contact adhesive and acetone.

1.3.5 Test Procedure


Clean the surfaces of the hard rubber and the foam rubber with acetone.
Join the foam rubber to the hard rubber sheets with the contact adhesive to form
a single overlap joint with an overlap length of 2.5 cm.
Using the marker pen, trace vertical lines along the overlap length on the joint as
indicated in Figure 1.19.
Load the joint by pulling both adherends on opposite directions and observe the
deformation of the joint in the overlap length region. This demonstration can be
performed in a classroom using a manually applied load. The same specimen can
also be used in a tensile machine, which will allow for the stress concentrations at
the ends of the overlap length to become more visible.
14 1 Simple Practical Demonstrations

Figure 1.19 Schematic representation of the vertical trace along the length of the joint.

Figure 1.20 Single lap joint in an unloaded state.

Figure 1.21 Single lap joint in a loaded state.

Observing the vertical lines made on the adhesive layer (see Figure 1.20) is a simple
method to determine the level of stress present along the bondline in an adhesive
joint. Figure 1.21 shows a loaded joint, and it is clear that the level of shear stress is
higher at the ends of the overlap length.
Figure 1.22 schematically shows the areas of the adhesive joint where the concen-
tration of stresses is greater, i.e. the edges of the joints.

Stress concentration

Figure 1.22 Schematic representation of stress concentration in an adhesive joint when


subjected to shear stresses.
1.4 Visual Identification of Defects in Adhesive Joints 15

1.4 Visual Identification of Defects in Adhesive Joints


1.4.1 Introduction
Because of poor storage conditions, manufacturing problems, large internal stresses,
or unexpected service loads, defects may appear in an adhesive layer or within
interfacial areas. Defects should be detected whenever possible as they can signif-
icantly impact the joint strength, leading to premature failure and compromising
structural integrity. Defect type, size, and location are three important factors
affecting the joint strength. Porosity, cracks, voids, detachments, presence of a
foreign object, poor curing, and poor adhesion are some of the defects that can be
observed in a poorly manufactured joint (see Figure 1.23).
These defects can be grouped into three major groups:

● Poor adhesion (poor bonding between the adhesive and the adherend), which
results from poor surface preparation or by the presence of contaminating sub-
stances in the adherend;
● Poor cohesive strength, resulting from incorrect adhesive formulation, poor mix-
ing, or insufficient adhesive curing;
● Voids and porosities that result from the presence of air bubbles, volatile release,
inadequate curing, thermal contraction, or application of the adhesive. This type
of defect is most easily detectable by non-destructive techniques.
Voids are usually created because of the presence of trapped gas/air bubbles
in the adhesive mixture, even before the adhesive is applied to the surface. Voids
in the adhesive layer also come from the incorrect pattern of adhesive applica-
tion on the bonding surface, which can cause air to trap inside the adhesive layer.
Figure 1.24 and Figure 1.25 show some of the good and bad practices associated
with the application of adhesives and the manufacture of bonded joints. Follow-
ing these recommendations will minimize the probability of having defects in an
adhesive joint.

The presence of voids leads to a decrease in joint strength, a decrease in the


adhered area, and an increase in the stress level within the adhesive layer. The
presence of voids leads to a decrease in joint resistance, a decrease in the adhered
area, and an increase in the stress level within the adhesive layer. Hence, a proper
Adherend

Weak adhesion

Void
Adhesive

Crack Porosity Poor cure


Unbound
Adherend

Figure 1.23 Types of defects that can be found in an adhesive joint.


16 1 Simple Practical Demonstrations

Good practice Bad practice

Figure 1.24 Good and bad practice in adhesive application.

Good practice Bad practice

Figure 1.25 Good and bad practice in top adherend application.

quality control procedure will examine the presence of voids in adhesive layers. If
air is trapped at the interface between the adhesive and the adherend, a disbonded
region will be created.
Discontinuities, voids, relative sliding between adherends, insufficient amounts
of adhesive, fracture, and indentations or dents are examples of defects that can be
identified by macroscopic observation of the bonding area. Visual inspection as a
non-destructive control method is a simple task that only allows a first identification
of the bond quality.
One of the main methods used to perform the quality control of adhesive joints is
visual control, not only at the time of manufacture but also after the execution of the
joint. While the visual inspection method is a simple approach used to perform the
quality control of adhesive joints, the inspection operator must be highly skilled and
experienced. Moreover, it is crucial to provide adequate light intensity, ensure the
correct viewing angle, and use the most suitable tools. The accuracy of this technique
is highly dependent on the quality of the supporting installation. Visible defects and
faults should be compared with reference images in inspection manuals to ensure
that they are within an acceptable range.
This type of control is appropriate for identifying defects or flaws that are notice-
able on the surface of the joint. In addition, geometric faults such as misalignment,
non-uniform adhesive thickness, incorrectly shaped fillets, etc., can also be visually
observed. Lack of excess adhesive or filleting at the edges of the bondline after man-
ufacture may be a sign of insufficient adhesion between the adherends or a poorly
secured bondline (thicker bondline).
1.4 Visual Identification of Defects in Adhesive Joints 17

1.4.2 Equipment
● Magnifying glass
● Metallic coin

1.4.3 Materials
● Examples of adhesive joints that are misaligned, porous, with “burnt” adhesive,
with non-uniform thickness, and with missing adhesive.

1.4.4 Safety Precautions


No hazards to report.

1.4.5 Test Procedure


In Figure 1.26, it is possible to observe the geometric misalignment of an adhesive
joint. It is clearly visible that the bottom adherend is not in the correct position,
while the correct position of the adherend is marked in red. These joint misalign-
ments cause stresses to be different from those expected for a given adhesive joint,
which, in addition to all the dimensional errors, can lead to serious constraints in
joint performance.
The correct curing process for an adhesive is always listed in the technical data
sheet provided by the supplier. It is very important to follow these indications
because the use of incorrect procedure (for example, too low temperature) might
lead to insufficient cure, and the strength of the joint will be lower than as designed.
On the other hand, if the curing temperature is higher, we can “burn” the adhesive
(see Figure 1.27). In fact, both excessive temperatures and long curing times may

Misaligned substrate

Correct substrate alignment

Figure 1.26 Adhesive joint with geometric misalignment of one of the adherends.
18 1 Simple Practical Demonstrations

Burned adhesive

Figure 1.27 Adhesive joint showing areas of burnt adhesive due to excessive curing
temperature.

Lack of adhesive

Figure 1.28 Adhesive joint missing adhesive in parts of the overlap area.

lead to a degradation of the polymeric chains, leading to a loss of chemical and


mechanical properties.
One of the most common defects observed in joint production is the lack of
adhesive at the edges (Figure 1.28). This defect can lead to premature failure of the
adhesive joint, as only a small part of the joint is being used to attain the strength for
which the joint was designed. This defect is mainly due to poor quality execution
of the adhesive joint, usually by an insufficient application of adhesive or poor
application of the adhesive along the length of the overlap. This defect may also be
associated with an inhomogeneous variation of the adhesive layer thickness if there
is no tight control of this dimension.
The tap test, like the visual test, is among the simplest NDT approaches used
in practice. In this test, the joint surfaces are tapped with a tool, as presented
in Figure 1.29. In our example, we will use a coin, but a hammer or even your
knuckles could be used instead. An operator will listen to the reflected sound wave
to determine whether the joint is qualified or not. Large unbound areas between
the joint and the adhesive or the presence of significant voids will visibly alter the
reflected sound. Voids or defects generate a resonant sound, whereas when there
is no defect, the sound is usually hollow. While effective in detecting the existence
of many defects, this approach is unable to provide information about the size or
1.5 Failure Analysis of Adhesive Joints 19

Figure 1.29 Detection of voids with the aid of a coin by the analysis of the sound emitted.

type of defects. Furthermore, if the defect is far from the surface, it will be difficult
to detect using the tap test. Once again, this test is closely related to the experience
of the operator.

1.5 Failure Analysis of Adhesive Joints

1.5.1 Introduction
The ultimate purpose of an adhesive joint is load transfer between the two bonded
components, maintaining its structural integrity under static and/or dynamic
stresses and adverse environmental conditions (temperature and humidity). It
therefore becomes fundamental to correctly assess the distribution of the stress
profile and, consequently, the failure modes induced in the bonded joints.
In the majority of failures in adhesive joints, it is possible to distinguish three dif-
ferent failure modes (Figure 1.30):
● cohesive breakage inside the adhesive,
● adhesive breakage at the interface between the adherend and the adhesive, and
● breakage of one of the adherends.
These three failure modes are schematically presented in Figure 1.30.
Adhesive failure occurs when there is poor surface preparation. This happens
when there is a loss of adhesion between the adhesive and the adherend. The bond
(chemical and mechanical) that should solidly connect the adhesive to the adher-
ent is somehow lost and there is a clear separation between these two materials at
the interface. When we have adhesive failure, it is possible to accurately determine
the strength of the adhesive layer using a variety of models that are based on the
mechanical properties of adhesive materials. The same is not true when we have
adhesive failure, as the interface properties are extremely difficult to determine and
may depend on several complex factors.
20 1 Simple Practical Demonstrations

Types of failure

Cohesive failure
(undesirable)

Joint before failure

Adhesive failure
Adhesive (undesirable)

Substrate failure
(desirable)

Figure 1.30 Schematic representation of the different failure modes in single overlap
bonded joints.

On the other hand, a joint must be designed so that the weakest element is the
adherend, i.e. failure never occurs through the adhesive. When this type of failure
occurs, it is known that the adhesive joint is designed to be stronger than the material
being joined. When failure occurs in the adherend, this does not necessarily mean
that the adherent will break cleanly, and the adhesive layer will remain intact. Often,
the adherent will instead yield and become permanently deformed (in the case of
metals) or delaminate (in the case of composites), and this can then lead to the failure
of the adhesive layer. Ultimately, a correctly designed and produced joint will be one
in which adherend failure occurs first, even if the adhesive itself becomes damaged
and fails as a result of this.
When an adhesive joint is manufactured using composite laminates, the situation
may be more complex, so it is advisable to use adherends that have surface layers
with fibers oriented parallel to the direction of stress, seeking to avoid interlaminar
failure of these layers.

1.5.2 Equipment
● Magnifying glass
● Protective gloves

1.5.3 Materials
● Fractured adhesive joints, showing adhesive, cohesive, and interfacial failures
● Adhesive joints with metallic and polymeric adherends (with and without defor-
mation)
● Composite adhesive joints

1.5.4 Safety Precautions


Gloves should be worn to avoid skin injuries caused by the sharp fibers that are
presented in the fracture composite materials.
1.5 Failure Analysis of Adhesive Joints 21

Figure 1.31 Adhesive joint with adhesive failure.

1.5.5 Test Procedure


This work consists in the careful observation of the fracture surfaces of different
adhesive joints. Ideally, the observation can be done with the naked eye, but in more
complex cases, more sophisticated equipment should be used, such as magnifying
glass or a microscope (optical or electron).
In Figure 1.31, an adhesive failure is observed, whereupon the adhesive does not
bond to one of the adherends, and the failure occurs at the interface between the
adhesive and the adherend. As already described, this type of failure is highly unde-
sirable. This sort of failure means that the surface preparation is not ideal, leading
to a premature failure of the adhesive joint.
A cohesive failure in the adhesive is demonstrated in Figure 1.32. Failure occurs
in the middle of the adhesive layer, demonstrating good adhesion of the adhesive
to the adherends. Although better than adhesive failure, this type of failure is also
undesirable in practical applications as the adhesive is still the weakest link within
the joint.
The adhesive joint shown in Figure 1.33 shows adherend failure. In other words, it
can be concluded that the joint is well designed, and the surface preparation is well
executed as the weakest element of the adhesive joint is now the adherend material
and not the adhesive layer or its interface. In this specific case, it is easily seen that
there is a great concentration of stresses at the edge of the adhesive joint overlap
coupled with massive plastic yielding of the polymeric adherend.
The same adhesive can be used to manufacture adhesive joints with metallic
adherends using hard steel. In this case, failure occurs within the adhesive, and,
unlike the joints bonding the polymeric material, there is no yielding of the metallic
adherends. However, some voids can still be noticed, suggesting that the adhesive
mixture or applications was not perfect. In this case, the surface preparation is also
22 1 Simple Practical Demonstrations

Figure 1.32 Adhesive joint with cohesive failure in the adhesive.

Figure 1.33 Adhesive joint with adherend failure.

appropriate because there is adhesion between the adhesive layer and the adherend
(Figure 1.34).
In Figure 1.35, showing a mixed failure, it is visible that the failure mechanism is
half cohesive and half adhesive. Occurrence of adhesive failure means that the sur-
face treatment can be improved in order to improve the adhesion, obtaining cohesive
failure.
In Figure 1.36, it is visible that adherend delamination occurs, as composite fibers
separate from the matrix material and become exposed. This type of failure is very
disadvantageous because it occurs in the areas where the peel stresses generated
1.5 Failure Analysis of Adhesive Joints 23

Voids

Figure 1.34 Cohesive failure in the adhesive layer, in metallic adhesive joints.

Adhesive failure

Figure 1.35 Mixed failure (cohesive and adhesive failure).


24 1 Simple Practical Demonstrations

Delamination

Figure 1.36 Example of delamination failure of composite joints.

by the adhesive layer are at the highest and the poor transverse strength of the
composite is overcome. In these cases, it is necessary to redesign the joint in order to
ensure that there is no delamination. This can be done, for example, by reinforcing
the overlapping area with fillets or chamfers.
25

Production and Testing

2.1 Bulk Specimens

2.1.1 Introduction
Multiple test methods are available to determine the strength of an adhesive.
These methods can be divided into two different techniques, which are tests of
neat resin/bulk specimens or tests carried out in a joint. The bulk specimens most
commonly used for adhesive testing are shaped as a “dog bone,” following diverse
standards for testing of plastic materials. The use of joints to characterize the
adhesive adds additional challenges to this process, such as the proper selection
of surface treatment of adherends (in order to ensure that the adhesive is properly
characterized) and to ensure that the stress field in the adhesive layer is as uniform
as possible. Because of this fact, the use of bulk specimens is generally preferred.
Bulk specimens can be manufactured by pouring or injecting adhesives. The injec-
tion technique consists in the injection of the adhesive directly in a mold with the
final shape (Figure 2.1). It allows us to avoid problems associated with machining
and cutting of the specimens, something that is especially hard when very ductile
adhesives (e.g. silicone adhesives) are used. The metallic mold is composed of top
and bottom parts and a middle frame with the final shape of the specimens. The
three parts are fitted together with screws, and it is the torque applied to these screws
that will control the pressure applied in the adhesive layer (pressure limited after the
three parts come in contact with each other). The main problem associated with this
technique is associated with the shrinkage of the adhesive during the curing process,
leading to important defects in the surface (e.g. voids).
The adhesive pouring technique consists of two main steps: the manufacture of a
bulk plate and the subsequent machining of the “dog bone” shape (Figure 2.2). This
technique is suitable for any type of adhesive and in any form (liquid, paste, or film),
allowing the production of adhesive plates without defects.

2.1.2 Adhesive Pouring Technique


The production of adhesive plates follows the French standard NFT76-142 that
describes the manufacture of plates in a mold with a silicon rubber frame under

Adhesive Bonding Technology and Testing, First Edition. Ricardo João Camilo Carbas,
Eduardo André Sousa Marques, Alireza Akhavan-Safar,
Ana Sofia Queirós Ferreira Barbosa, and Lucas Filipe Martins da Silva.
© 2023 WILEY-VCH GmbH. Published 2023 by WILEY-VCH GmbH.
26 2 Production and Testing

Figure 2.1 Tensile specimens produced with injecting techniques.

Figure 2.2 Tensile specimens produced with adhesive pouring techniques.

high pressure (2MPa). The different elements necessary to obtain adhesive plates
with high quality are shown in Figure 2.3. A special metallic mold with an internal
silicone frame is used, and the adhesive should fill this silicone frame with an
excess of 5% in volume. This excess amount will flow out from the mold cavity and
draw with it voids and bubbles. When pressure is applied to the mold, the internal
silicone frame will expand sideways and generate a hydrostatic pressure in the plate,
further ensuring that voids are removed and ensuring a consistently compressed
material. Moreover, it is this silicone frame that controls the final thickness of the
plate.

2.1.3 Metallic Mold


The French standard (NF T 76-142) suggests a generic dimension for the metallic
mold used to obtain good-quality adhesive plates. Figure 2.4 schematically shows a
metallic mold suitable to obtain these plates. The mold is composed of a base and a
2.1 Bulk Specimens 27

Figure 2.3 Schematic representation of pouring technique.

Mould
Base and lid
235
7 195

7
130
90

Metalic frame
A–A
14
1

A
20

ø7 H14 20 40 20 37,5 10
A
235

B–B
1

7
14
10

18 8 B
10 7
7

13

20 B 20
25
90

Figure 2.4 Technical drawing of a metallic mold used in the pouring technique
(dimensions in mm).
28 2 Production and Testing

Figure 2.5 Removal of dust and particles from the mold surface.

lid with the same dimensions, showing a working area of 195 × 90 mm2 . It is within
this working area that the silicone frame should be inserted. In order to ensure
that the silicone remains fixed during the curing process, the working area must
be restricted by a metallic frame composed of four metal beams fastened together.
The surfaces that come in contact with the adhesive must be prepared in advance.
Contaminants on the metal surface must be removed to ensure good adhesion of the
adhesive through manual cleaning with a sandpaper, followed by degreasing of the
surface using acetone (Figure 2.5).
Before closing the mold, the different parts of the mold should be covered by a thin
layer of release agent to facilitate the remotion of the plate after curing (Figure 2.6).
The release agent should be properly selected as a function of the adhesive being
used as different adhesives react differently to the mold release agents available in
the market.
The different parts should be mounted, and the screws are properly tightened to
ensure that all parts remain in position during the pressure application. Before the
application of the adhesive, the silicone frame should only be applied to the mold
after the release agent is fully cured (Figure 2.7). Please note that the silicone frame
does not require coating of the release agent because most adhesives do not readily
2.1 Bulk Specimens 29

Figure 2.6 Application of mold release agent.

Figure 2.7 Assembly of different parts of the mold and positioning of the silicone frame.
30 2 Production and Testing

bond well to silicone. Moreover, no contact should be allowed between the adhesive
and the uncured mold release agent as this will damage the adhesive.
The silicone frame has two main purposes. The first is to control the final thickness
of the plate, whereas the second is the application of a hydrostatic pressure to the
adhesive during the curing process, ensuring the removal of any voids.
Generally, thicknesses of 2 mm are often used, and the maximum internal dimen-
sions of the cavity where the adhesive will be deposited are 140 × 65 × 2 mm3 , ensur-
ing the manufacture of defect-free plates. The silicone rubber that is typically used is
a room temperature vulcanizing (RTV) silicone with a hardness of about 50 Shore.

2.1.4 Adhesive Application


The adhesive is applied to the cavity formed by the silicone frame in a quantity that
is 5% of excess of the volume of the cavity. For two-component adhesives supplied
in separate containers, the mixture of the resin and hardener is a very important
process because voids can be introduced (Figure 2.8a). To avoid these defects, the
mixture should be performed using a high-speed centrifuge machine, an ultrasonic
mixer, or with the assistance of a vacuum chamber (Figure 2.8b). Moreover, to weight
each component, precision scales should be used because the incorrect ratio of hard-
ener to resin can lead to vastly different mechanical properties after curing or even
lead to a situation where the adhesive never fully cures. In some cases, two-part
adhesives are supplied in cartridges (one and two components), and the mixture is
carried out with the use of an appropriate nozzle (Figure 2.9).
The mixed adhesive should be deposited within the silicone frame in a
well-controlled manner, with closely clumped beads and then uniformly spread to
avoid the introduction of voids.

(a) (b)

Figure 2.8 Equipment used to ensure proper mixing of adhesives supplied in separated
containers: (a) precision scales and (b) high-speed centrifuge. Source: IndiaMART InterMESH
Ltd.
2.1 Bulk Specimens 31

(a)

(b)

Figure 2.9 Two different techniques to apply the adhesive: (a) with the use of a nozzle and
(b) with the use of a spatula.

The closure of the mold also requires special attention to reduce the air trapped
within the plate. This is achieved by closing the mold in a continuous rotational
movement (Figure 2.10). A direct vertical translation of the mold cover should be
avoided as it minimizes paths for the release of trapped air.

2.1.5 Curing Procedure


The closed mold is subjected to high pressure, and this can be achieved in a hot
plate press, where both the pressure and the temperature can be precisely controlled
to reduce the production times and ensure consistency (Figure 2.11). The heating
and cooling ramps must also be properly controlled in order to ensure a uniform
temperature within the mold, something that is fundamental to reduce the thermal
gradients that will generate large residual thermal stresses.
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“You want to know how old Henry C. Terry is,” promptly said Reese.
Then plainly puzzled, he shook his head and went on to a question as to
what was the floor covering. The next question was: “Where did I do my
first newspaper work?”
He gave correctly the answer. The last slip Reese took in his hand, but
did not open it. He handed it back and directed the writer to hold it. Then
Reese said:
“Emma Drew was your mother’s maiden name.”
The answer to the first five questions had been given in a room adjoining
the court, but for the last Reese walked into the courtroom and gave his
answer in the presence of the judge and jury.
Judge Rosalsky wrote several questions, as follows:
“What was the ruling in the Shelly case?”
“How much money have I in the bank?” and
“What is the name of my favorite school-teacher?”
The demonstrator not only told what the questions were, but gave the
correct replies. Reese is seventy-four years old.
“I don’t know myself how I do it,” he said. “The answers just sort of
flash on my brain as a picture, just as ordinary objects are seen through the
eye.”

Kaiser’s Big Cannon Can’t Make Raindrops.


So many days during the last two months have been rainy or cloudy that
a great many people are led to believe that so much wet weather is owing to
the war in Europe. “Our heavy rainfall is probably caused by so much firing
over there,” is a remark frequently heard. Indeed, as long as man can
remember, it has been a theory accepted by many that constant or heavy
explosions in the air will produce rainfall. Tests of this kind have been made
in various parts of the country—more often in the west and southwest—and
sometimes with evident success, yet skeptics were quick to say: “Shucks, it
was time they had a shower, anyway.”
Now let us see how the ancients looked at this question. Almost since
the beginning of history there has been a theory—a silly one, says one
scientist—that battles caused rain. Battles, not explosives, observe, for in
the early centuries, A. D., there were no gunpowder or similar explosives.
“Banish the thought,” says Forecaster Pennywitt, of the United States
Weather Bureau, in discussing the question of explosives and rainfall.
“There never was a more absurd idea. Not in all the history of the world is it
recorded that human endeavor wrung rain from the skies, either
intentionally or unknowingly. Rain falls by the will of nature only, and the
influence of man over nature, in so far as producing rain is concerned, does
not exist.
“None of men’s activities on earth has the slightest effect on the rainfall.
If nature decrees it shall rain, then rain it will; no other power or force can
bring precipitation.
“Almost since the beginning of history there has been a silly theory that
battles caused rain. This was the case even before gunpowder came into
use. The Greek writer, Plutarch, as far back as the year 150 A. D., held the
belief that the glitter and clash of the sabers of the ancient Greek and
Roman warriors on the field of honor produced rain. He believed it because
it generally rained after every battle. As a matter of fact, it had to rain after
every battle, because they fought only on clear days in those times; and,
besides, it always rains once every three days in the year, according to
average.
“After gunpowder became an instrument of destruction, rains during
time of war were blamed on it. Even the United States government has
shared this belief that powder will produce rain, and it wasted thousands of
dollars trying to make it rain in Texas. Similar experiments were made in
Europe several years ago, and in France one scientist thought that by
employing the explosive he could transform hail into more harmless rain.
“Strange as it may seem to a good many people, there has been less than
a normal rainfall in western Pennsylvania and other eastern districts during
the last six months.”

Bees Settle in a Mail Box.


The wanderlust of summer got into the blood of a swarm of bees
belonging to Leo Nickoli, 448 Bellaire Avenue, Kansas City, Mo. They
circled in the air and flew away. Mr. Nickoli followed.
The awning in front of the drug store of the Klee Drug Company first
attracted the bees. But finding no place to alight there, the bees transferred
their attentions to a mail box near by. In a moment the box was the center of
the swarm, who were preparing to settle down among the letters.
Mr. Nickoli, however, had different plans. With a hive baited with honey
comb, he began coaxing the bees into a new home. A crowd of two hundred
persons watched his operation, which lasted several hours.

Aged Preacher Finds His Long Lost Sister.


An only sister, whom he had not seen nor heard from for more than
forty-five years, and whom he believed to be dead, has been found by
Reverend W. H. H. Ruble, of Harrison, Ark., and immediately after the
locating of the long-lost sister, he has received news that sight has been
restored to the woman who has been blind for many years, as a result of
cataract.
Reverend Ruble’s sister is Mrs. E. J. Willis, of Knoxville, Tenn. She is
ninety-two years of age, and was last seen by her brother more than forty-
five years ago in Cleveland, a small town of Tennessee. As many people do,
the brother and sister kept in touch for a time, but gradually ceased writing,
until each had changed address and the old addresses were forgotten.
Receiving no word for years, each believed the other to be dead, until
last January, when the annual conference of the M. E. Church was held in
Harrison, Ark. At that time Reverend Ruble met Reverend Murphy, a
delegate, who told him of the whereabouts of Chaplain J. A. Ruble, of the
Old Settlers’ Home in Johnson City, to whom Reverend Ruble wrote,
believing that the chaplain might be his nephew. The belief was true, and
the letter from Harrison was forwarded to Mrs. Willis, who was overjoyed
when she wrote again to her brother, the first time in nearly half a century.

Arizona Girl Carries Mail on Horse.


Miss Matilda Sorey, of Higley, Ariz., may not be the only girl in the
United States who carries mail on a R. F. D. route, but she is probably the
only one who does so on horseback. When a new route was established out
of Higley, Miss Sorey, who is just twenty-one years old, was appointed
carrier. Her friends supposed she would use a horse and buggy, but, instead,
she covers the route six days a week on her handsome gray saddle horse.
She carries the mail in a sack swung over the pommel of her cowboy
saddle.

Didn’t Even Have a Barrel.


A short time ago C. J. Debes, who lives on a farm a few miles south of
Hagerman, N. M., arose early, as was his custom, and, after lighting his
gasoline stove and placing his kettle on, sauntered out through the
delightful morning air to feed his stock, without changing his night robe for
the more substantial clothing of the day.
Debes being a bachelor, and there being no near neighbors, everything
went well with him until he started to return to his house and found it
almost consumed by fire. His predicament seemed precarious, when the
neighbors, seeing the flames, rushed to the scene. Debes, however, took
refuge in the barn until a friendly neighbor brought in some heavier
raiment. The gasoline stove had exploded and enveloped the entire building
in flames, making quick work of its destruction.

No Government Reward for Passenger Pigeon.


Recent widespread newspaper accounts to the effect that the United
States Department of Agriculture is offering ten thousand dollars reward to
the person finding a passenger or “wood”-pigeon nest containing two eggs,
resulted in hundreds of letters being sent to the department.
The report is not based upon facts, as the department has offered no such
reward, and there is every reason to believe the passenger pigeon which
formerly roamed the country in flocks of millions is extinct. In 1910 about
one thousand dollars in rewards was offered by Clark University for the
first undisturbed nests of the passenger pigeon to be found in the United
States. This was a great stimulus to action. The hunt for this pigeon was
fruitless. The offer of rewards was renewed for several years, until it was
fully established that the pigeon was extinct.
The passenger pigeon up to 1885 ranged the American continent east of
the Rocky Mountains. The mourning dove has often been mistaken for the
passenger pigeon, which in a general way it resembles. However, this bird
is quite distinct from the passenger pigeon; it is shorter and has different
color markings.
The press reports stated that the now extinct passenger pigeon was
valued because of its usefulness in destroying the gipsy moth and other
moths and pests which are doing millions of dollars of damage. Although
the preservation of this pigeon is much to be desired, it would be of
absolutely no value in eliminating the gipsy moth, as the pigeons are almost
entirely vegetarian in their diet.

Wounded Dog Returns Home.


A dog belonging to Edward Dougherty, of Spring Grove, Pa., was shot
through the head twice with a thirty-eight-caliber revolver by Dougherty.
The dog lay on the same spot for seven days and seven nights, but on the
beginning of the eighth day he came back to his old home, hardly able to
drag himself along. After being fed and given water to drink, the dog
seemed to be all right.
The dog ate eggs from the nests in Dougherty’s henhouse before his
punishment and since his extraordinary experience he has not eaten one
egg. Mr. Dougherty is sure he put two bullets through the dog’s brain.

Muskrat and Trout Battle.


Lew McQuiston, a well-known angler of Bellefonte, Pa., witnessed a
unique battle a few days ago between a muskrat and a two-foot trout.
McQuiston went to Spring Creek shortly before dusk to try and land
some big trout. While whipping the stream, he saw something doing on the
other side of the creek, about sixty feet away from where he was standing.
In the quickly gathering shadows it was hard to tell at first what it was, but
after closer inspection he saw that it was a mammoth trout and a muskrat.
They were engaged in mortal combat, and they slashed around through
the water until it was churned into foam. Then the muskrat managed to get
out on the bank, pulling the trout along with it. But the big trout seemed to
be able to fight on land as well as in the water, flopping around and holding
on to the muskrat’s nose until they finally both fell back into the water.
Then there was another lashing and foaming, and the noise died away. A
few ripples told that the struggle was ended.
McQuiston looked around in the water for evidence of who had won the
battle, but found neither the muskrat or the trout. He does not know whether
it was a fight to the finish or a draw.

Tongue Fenders Demanded.


Tongue fenders for salted-peanut vending machines. That’s the latest
slogan of Montclair, N. Y., which already has put a legal muffler on barking
dogs and crowing roosters. It was proposed by Health Commissioner James
McDonough after he saw a small boy thrust his tongue into a cup container
of a vending machine to get the “crumbs.”

Finds Pennies in Turtle.


Roy Bowsher, of Ashville, Ohio, went fishing last week and caught a
turtle, which he sold to C. R. Cook, proprietor of a saloon. When Cook
opened the turtle, preparatory to serving it on his lunch counter, he found
two hundred and thirty-four pennies in it.

The Nick Carter Stories


ISSUED EVERY SATURDAY BEAUTIFUL COLORED COVERS
When it comes to detective stories worth while, the Nick Carter Stories
contain the only ones that should be considered. They are not overdrawn
tales of bloodshed. They rather show the working of one of the finest minds
ever conceived by a writer. The name of Nick Carter is familiar all over the
world, for the stories of his adventures may be read in twenty languages. No
other stories have withstood the severe test of time so well as those
contained in the Nick Carter Stories. It proves conclusively that they are
the best. We give herewith a list of some of the back numbers in print. You
can have your news dealer order them, or they will be sent direct by the
publishers to any address upon receipt of the price in money or postage
stamps.
730—The Torn Card.
731—Under Desperation’s Spur.
732—The Connecting Link.
733—The Abduction Syndicate.
738—A Plot Within a Plot.
739—The Dead Accomplice.
746—The Secret Entrance.
747—The Cavern Mystery.
748—The Disappearing Fortune.
749—A Voice from the Past.
752—The Spider’s Web.
753—The Man With a Crutch.
754—The Rajah’s Regalia.
755—Saved from Death.
756—The Man Inside.
757—Out for Vengeance.
758—The Poisons of Exili.
759—The Antique Vial.
760—The House of Slumber.
761—A Double Identity.
762—“The Mocker’s” Stratagem.
763—The Man that Came Back.
764—The Tracks in the Snow.
765—The Babbington Case.
766—The Masters of Millions.
767—The Blue Stain.
768—The Lost Clew.
770—The Turn of a Card.
771—A Message in the Dust.
772—A Royal Flush.
774—The Great Buddha Beryl.
775—The Vanishing Heiress.
776—The Unfinished Letter.
777—A Difficult Trail.
782—A Woman’s Stratagem.
783—The Cliff Castle Affair.
784—A Prisoner of the Tomb.
785—A Resourceful Foe.
789—The Great Hotel Tragedies.
795—Zanoni, the Transfigured.
796—The Lure of Gold.
797—The Man With a Chest.
798—A Shadowed Life.
799—The Secret Agent.
800—A Plot for a Crown.
801—The Red Button.
802—Up Against It.
803—The Gold Certificate.
804—Jack Wise’s Hurry Call.
805—Nick Carter’s Ocean Chase.
807—Nick Carter’s Advertisement.
808—The Kregoff Necklace.
811—Nick Carter and the Nihilists.
812—Nick Carter and the Convict Gang.
813—Nick Carter and the Guilty Governor.
814—The Triangled Coin.
815—Ninety-nine—and One.
816—Coin Number 77.
NEW SERIES
NICK CARTER STORIES
1—The Man from Nowhere.
2—The Face at the Window.
3—A Fight for a Million.
4—Nick Carter’s Land Office.
5—Nick Carter and the Professor.
6—Nick Carter as a Mill Hand.
7—A Single Clew.
8—The Emerald Snake.
9—The Currie Outfit.
10—Nick Carter and the Kidnaped Heiress.
11—Nick Carter Strikes Oil.
12—Nick Carter’s Hunt for a Treasure.
13—A Mystery of the Highway.
14—The Silent Passenger.
15—Jack Dreen’s Secret.
16—Nick Carter’s Pipe Line Case.
17—Nick Carter and the Gold Thieves.
18—Nick Carter’s Auto Chase.
19—The Corrigan Inheritance.
20—The Keen Eye of Denton.
21—The Spider’s Parlor.
22—Nick Carter’s Quick Guess.
23—Nick Carter and the Murderess.
24—Nick Carter and the Pay Car.
25—The Stolen Antique.
26—The Crook League.
27—An English Cracksman.
28—Nick Carter’s Still Hunt.
29—Nick Carter’s Electric Shock.
30—Nick Carter and the Stolen Duchess.
31—The Purple Spot.
32—The Stolen Groom.
33—The Inverted Cross.
34—Nick Carter and Keno McCall.
35—Nick Carter’s Death Trap.
36—Nick Carter’s Siamese Puzzle.
37—The Man Outside.
38—The Death Chamber.
39—The Wind and the Wire.
40—Nick Carter’s Three Cornered Chase.
41—Dazaar, the Arch-Fiend.
42—The Queen of the Seven.
43—Crossed Wires.
44—A Crimson Clew.
45—The Third Man.
46—The Sign of the Dagger.
47—The Devil Worshipers.
48—The Cross of Daggers.
49—At Risk of Life.
50—The Deeper Game.
51—The Code Message.
52—The Last of the Seven.
53—Ten-Ichi, the Wonderful.
54—The Secret Order of Associated Crooks.
55—The Golden Hair Clew.
56—Back From the Dead.
57—Through Dark Ways.
58—When Aces Were Trumps.
59—The Gambler’s Last Hand.
60—The Murder at Linden Fells.
61—A Game for Millions.
62—Under Cover.
63—The Last Call.
64—Mercedes Danton’s Double.
65—The Millionaire’s Nemesis.
66—A Princess of the Underworld.
67—The Crook’s Blind.
68—The Fatal Hour.
69—Blood Money.
70—A Queen of Her Kind.
71—Isabel Benton’s Trump Card.
72—A Princess of Hades.
73—A Prince of Plotters.
74—The Crook’s Double.
75—For Life and Honor.
76—A Compact With Dazaar.
77—In the Shadow of Dazaar.
78—The Crime of a Money King.
79—Birds of Prey.
80—The Unknown Dead.
81—The Severed Hand.
82—The Terrible Game of Millions.
83—A Dead Man’s Power.
84—The Secrets of an Old House.
85—The Wolf Within.
86—The Yellow Coupon.
87—In the Toils.
88—The Stolen Radium.
89—A Crime in Paradise.
90—Behind Prison Bars.
91—The Blind Man’s Daughter.
92—On the Brink of Ruin.
93—Letter of Fire.
94—The $100,000 Kiss.
95—Outlaws of the Militia.
96—The Opium-Runners.
97—In Record Time.
98—The Wag-Nuk Clew.
99—The Middle Link.
100—The Crystal Maze.
101—A New Serpent in Eden.
102—The Auburn Sensation.
103—A Dying Chance.
104—The Gargoni Girdle.
105—Twice in Jeopardy.
106—The Ghost Launch.
107—Up in the Air.
108—The Girl Prisoner.
109—The Red Plague.
110—The Arson Trust.
111—The King of the Firebugs.
112—“Lifter’s” of the Lofts.
113—French Jimmie and His Forty Thieves.
114—The Death Plot.
115—The Evil Formula.
116—The Blue Button.
117—The Deadly Parallel.
118—The Vivisectionists.
119—The Stolen Brain.
120—An Uncanny Revenge.
121—The Call of Death.
122—The Suicide.
123—Half a Million Ransom.
124—The Girl Kidnapper.
125—The Pirate Yacht.
126—The Crime of the White Hand.
127—Found in the Jungle.
128—Six Men in a Loop.
129—The Jewels of Wat Chang.
130—The Crime in the Tower.
131—The Fatal Message.
132—Broken Bars.
133—Won by Magic.
134—The Secret of Shangore.
135—Straight to the Goal.
136—The Man They Held Back.
137—The Seal of Gijon.
138—The Traitors of the Tropics.
139—The Pressing Peril.
140—The Melting-Pot.
141—The Duplicate Night.
142—The Edge of a Crime.
143—The Sultan’s Pearls.
144—The Clew of the White Collar.
145—An Unsolved Mystery.
146—Paying the Price.
147—On Death’s Trail.
148—The Mark of Cain.
Dated July 17th, 1915.
149—A Network of Crime.
Dated July 24th, 1915.
150—The House of Fear.
Dated July 31st, 1915.
151—The Mystery of the Crossed Needles.
Dated August 7th, 1915.
152—The Forced Crime.
Dated August 14th, 1915.
153—The Doom of Sang Tu.
Dated August 21st, 1915.
154—The Mask of Death.
Dated August 28th, 1915.
155—The Gordon Elopement.
Dated Sept. 4th, 1915.
156—Blood Will Tell.

PRICE, FIVE CENTS PER COPY. If you want any back numbers of our
weeklies and cannot procure them from your news
dealer, they can be obtained direct from this office. Postage stamps taken
the same as money.

STREET & SMITH, Publishers, 79-89 Seventh Ave., NEW YORK CITY
*** END OF THE PROJECT GUTENBERG EBOOK NICK CARTER
STORIES NO. 155, AUGUST 28, 1915: THE GORDON
ELOPEMENT; OR, NICK CARTER'S THREE OF A KIND ***

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