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Graduate Studies Legacy Theses

2002

Rotational molding of a polyethylene resin:

preliminary results on the effects of molding
conditions on the molded part characteristics

Han, Yuze

Han, Y. (2002). Rotational molding of a polyethylene resin: preliminary results on the effects of
molding conditions on the molded part characteristics (Unpublished master's thesis). University
of Calgary, Calgary, AB. doi:10.11575/PRISM/12034
http://hdl.handle.net/1880/42485
master thesis

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 University of Calgary

Rotational molding of a polyethylene resin:

preliminary results on the effects of molding
conditions on the molded part characteristics

By

Yuze Han

A THESIS

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D E P A R T M E N T OF C H E M I C A L A N D P E T R O L E U M ENGINEERING

CALGARY, ALBERTA

N O V E M B E R , 2002
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 ABSTRACT

The rotational molding industry is experiencing a rapid development. The process

involves powder tumbling, melting, and distributing of polymer melt and cooling to form

a solid part. The main concern in this work is to gain a better understanding of how

processing conditions affect powder densification in the rotational molding process.

The uni-axial bench-scale molding machine built in our laboratory is used for

studying the densification process. A n experimental procedure was set in place to ensure

proper control of molding conditions. The degree of densification achieved during

molding was determined based on the density of the molded part and bubble content in

the molded part. Density measurements were performed using an electronic densimeter

MD-200s, for which, larger volume sample part gives a more accurate result. Oven

temperature was found to have significant effects on the density profiles. Higher oven

temperature causes larger variations in the density with the axial position in the molded

parts. Small variations in the molding heating time also have important effects on the

density profiles. The powder sizes were found to have a definite effect on the density of

the molded parts. Powders with high fine particle content produced parts with lower

density and higher bubble content. Bubble distribution along the thickness reflects the

temperature changes experienced during molding cycle. Additional experimental work

will be needed to confirm some of the results presented in this work.

iii
 ACKNOWLEDGEMENT

I would like to thank my supervisor, Dr. Celine T. Bellehumeur, for having given

me the opportunity to work under her supervision. I very much appreciate her continuous

financial support and constructional guidance during my work.

This research would not have been possible without the help of many people.

These include: Mr. Derek Verhegge for building and repairing the rotational machine,

Mr. Bruce Miles for installing the data acquisition system. I am indebted to Mr. Sebastian

Kosciolek, Ms. Maricar Castillo, and Ms. Amy Wong for conducting rotational molding

experiments and part analysis which shed light to my own experiments and discussions. I

want to thank Mr. Wen Lin, Ms. Grace (Rong) Guo, and Ms. Qian Sun for assistant in

using some instruments and meaningful discussions during the whole research term. I

also thank Mr. Chetan Anand.

I am thankful to N O V A Chemicals Corporations for supplying the resins used in

this work. The financial support from the Department of Chemical and Petroleum

Engineering is also very appreciated.

I would also like to thank the faculty, staff and fellow graduate students at the

Department of Chemical and Petroleum Engineering for making my studies at the

University of Calgary so memorable and pleasant.

Last but not the least, I would like to thank my wife for her hard working and

contribution to the family during my study.

iv
To my wife

V
 TABLE OF CONTENTS

ABSTRACT iü

ACKNOWLEDGEMENT iv

DEDICATION v

T A B L E S OF CONTENTS vi

LIST OF T A B L E S ix

LIST OF FIGURES x

C H A P T E R ONE. INTRODUCTION 1

1.1 The Rotational Molding Process 1

1.2 The Material Used in Rotational Molding 3

1.3 The Machinery 4

1.4 The Molds 5

1.5 The Product 5

1.6 The Advantages and Disadvantages of Rotational Molding 6

1.7 Research Objective and Thesis Outline 7

C H A P T E R TWO. L I T E R A T U R E REVIEW 8

2.1 Simulation of Heat Transfer in Rotational Molding Process 8

2.2 Powder Sintering 10

2.3 Polymer Melt Densification and Bubble Removal 12

2.4 Effect of Powder Properties on the Rotational Molding Process and

Properties of Molded Parts 14

vi
2.5 Effect of Additives on the Rotational Molding Process and Properties

of Molded Parts 16

2.6 New Processes and New Products of Rotational Molding 18

C H A P T E R THREE. E X P E R I M E N T A L 21

3.1 Rotational Molding Experiments 21

3.2 Material Properties 24

3.3 Powder Characterization 24

3.4 Molded Part Characterization 25

3.4.1 Thickness Measurement of Molded Parts 25

3.4.2 Density Measurement of Molded Parts 25

3.4.3 Bubble Size Distribution 27

3.5 Experimental Procedures 27

C H A P T E R FOUR. RESULTS A N D DISCUSSIONS 31

4.1 Effect of Mold Characteristics on the Molding Cycles 31

4.2 Description of the Molding Cycle 31

4.3 Effect of Oven Temperature on the Molding Cycle 33

4.4 Molded Part Properties 36

4.4.1 Thickness Distribution 37

4.4.2Density of the Molded Parts 40

4.5 Bubble Size and Bubble Distribution 46

vii
C H A P T E R FIVE. CONCLUSIONS 54

REFERENCES 56

APPENDICES

E X P E R I M E N T A L PROCEDURES 62

UNI-AXIAL BENCH-SCALE MOLDING MACHINE 62

P R O C E D U R E FOR RS L A B 40 64

CUTTING R O T O M O L D E D S A M P L E S FOR TESTING THICKNESS 66

TESTING R O T O M O L D E D S A M P L E S FOR THICKNESS 66

CUTTING R O T O M O L D E D S A M P L E S FOR DENSITY M E A S U R E M E N T S .66

DENSITY M E A S U R E M E N T S 67

DETERMINING B U B B L E S IN THE R O T O M O L D E D PARTS 67

PARTICLE SIZE DISTRIBUTION (ASTM D 1921-96) 68

O V E N T E M P E R A T U R E CONTROL A N D O V E N

T E M P E R A T U R E DISTRIBUTION 69

viii
 LIST OF TABLES

Table 1. The Properties of Rotational Molding Material 24

Table 2. Oven Temperature and Corresponding Preset Temperature 29

Table 3. Oven Temperatures and Corresponding Removal Temperatures 30

Table 4. Absolute Error on the Density Measurements 40

Table 5. Repeatability of Density Measurement 70

Table 6. Repeatability of Density Measurement 71

ix
 LIST OF FIGURES

Figure 1 Rotational Molding Process 2

Figure 2 Effect of Particle Size on Properties 16

Figure 3 Bench Scale Rotational Molding Machine 23

Figure 4 Particle Size Distribution of Experimental Material 26

Figure 5 Sample Cutting Scheme for Thickness, Bubble and

Density Measurements 28

Figure 6 Effect of Mold Color on Molding Cycle Time 32

Figure 7 Molding Cycle and Oven Temperature (250°C) 33

Figure 8 Molding Cycle and Oven Temperature (350°C) 34

Figure 9 Molding Cycle and Oven Temperature (425°C) 35

Figure 10 Thickness Profile in the Molded Parts (40-50mesh) 38

Figure 11 Thickness Profile in the Molded Parts (powder as received) 39

Figure 12 Density Profile of Molded Parts (40-50mesh) 42

Figure 13(a) Density Profile in the Molded Parts (350°C) 43

Figure 13(b) Molding Cycle for Different Maximum Inside Air Temperature....43

Figure 14(a) Density Profile in the Molded Parts (425°C) 44

Figure 14(b) Molding Cycle for Different Maximum Inside Air Temperature....44

Figure 15(a) Effect of Particle Size on Molded Part Density 45

Figure 15(b) Effect of Particle Size on Molding Cycle 45

x
Figure 16 Optical Micrograph of a Thin Cross Section of a Molded Part 48

Figure 17 The Effect of Oven Temperature on the Number of Bubbles 49

Figure 18 Bubble Size Distribution in the Molded Parts 50

Figure 19 Bubble Size Distribution in the Molded Parts 51

Figure 20 The Effect of Particle Size on Bubble Size

Distribution in the Molded Parts 52

Figure 21 The Temperature Responses for Different pbl Values 72

Figure 22(a) Temperature Profiles at Different Positions 73

Figure 22(b) The Average Temperature of the Oven (with mold in) 73

xi
 1

CHAPTER ONE

INTRODUCTION

1.1 The Rotational Molding Process

Rotational molding is a process for producing hollow plastic articles. The process

involves powder mixing, heating and melting of powder particles to form a homogeneous

polymer melt, as well as cooling and solidification. Generally, rotational molding process

consists of the following stages (Figure 1).

(i) The polymer, usually in powder form, is placed in one half of a hollow metal mold.

The amount of powder required is determined by the thickness of articles to be

produced.

(ii) The charged mold is closed and placed inside an oven for heating. Depending on the

size of moldings, a vent-pipe is usually incorporated in the mold to allow some air in

when the mold is being cooled. The mold is then rotated bi-axially in two

perpendicular planes. The optimal heating time and oven temperature are usually

determined by trial and error. The rotating speeds and speed ratio of major and minor

axes are also determined based on experience. The bi-axial rotation ensures uniform

distribution of the powder over the entire inner surface of the mold. When the

temperature of the inner surface reaches the melting point of the polymer, the powder

starts to stick on the mold surface. The mold is heated and rotated bi-axially until all

powder has melted onto the mold surface. As the powder particles adhere to the mold

surface, pockets of air get trapped within the melt and form bubbles. The mold is
 (3) Cooling Cycle (4) Molded part unloading

Molded part
Rotating and cooling

1—r
c3>

Figure 1 Rotational Molding Process (Crawford [1])

 3
further heated to promote the dissolution of these bubbles into the melt. The

phenomena of bubble formation and dissolution lead to an increase in the melt density

(densification).

(iii) After a sufficient amount of time has been allocated to the densification process, the

mold is moved to a cooling area. Cooling is carried out by forced air, water spray or

water shower.

(iv) Once the molding part reaches an easy handling temperature, the part is removed

and the mold is charged for the next molding.

From the above four steps, it is seen that processes such as heat transfer, melting and

fusion of powder (also referred to as sintering), dissolution of bubbles and solidification

are fundamental phenomena of rotational molding process. The performance of molded

parts is controlled in part by the degree of powder densification achieved during the

heating cycle and by the melt solidification process.

1.2 The Materials Used in Rotational Molding

Polyethylenes are the most widely used resins in the rotational molding industry since

they have good flow properties, thermal stability, impact strength and a very wide range

of properties by polymerization of ethylene and by co-polymerization of ethylene-butene,

ethylene-hexene or ethylene-octene. By physical modifications, such as multiple layers,

the performance of molded parts can be improved. Other materials such as

polypropylene, polyamides (nylons), polycarbonate, poly(acrylonitrile-butene-styrene)

(ABS), polyvinychloride (PVC) can also be rotationally molded. However, due to the
 4
limitations of these materials (very high viscosity, or poor thermal stability), they account

for less than 20% of all parts produced by rotational molding.

1.3 The Machinery

There is a wide range of machines that have been used for rotational molding.

The basic requirements of a rotational molding machine are that the mold is first heated

and then cooled whilst it is rotating, usually in a bi-axial manner. Heating methods

available include forced hot air convection, oil heated jacket, infrared radiation and open

gas fire. Hot air ovens are the most commonly used in rotational molding machines. Air

under forced convection can provide good coverage and therefore almost uniform heating

of all but molds with extremely complex geometric shapes. Cooling is usually performed

by forced air from a fan, water mist or water shower. A combination of these is most

commonly used to achieve good part performance and for economical reasons. Air-

cooling will usually be very slow and lead to long cycle times. Water-cooling usually

cools too fast and causes part warpage and shrinkage. Internal cooling can also be used to

provide more uniform cooling from the inner surface of the part to control distortion.

Rotating is realized by means of either variable speed drives or fixed speed drives with

inter-changeable gears or chain sprockets. The speed of rotation is slow, typically in the

range of 4 to 25 rpm and the ratio of rotation between the main and minor ranges varies

from 10:1 to 1:10.

 5
1.4 The Molds

Molds used in rotational molding are usually thin-walled, light-weight and relatively

low-cost in comparison with injection or blow molding. The choice of material and

method of production will depend on the size, complexity, surface finish requirement,

number of molds and the production run anticipated. The most commonly used materials

include steel and aluminum. Typically aluminum molds are thicker than steel to

compensate for the low strength of aluminum. The mold thickness is also affected by the

mold's ability to withstand the repeat thermal cycle found in rotational molding. Molds

are not normally designed to withstand pressure so that a vent pipe is usually

incorporated to allow equilibrium between the oven atmosphere and the air inside the

mold and to allow any emission to escape.

1.5 The Product

By the nature of rotational molding, the process is best suited to the production of

hollow items. The first products of rotational molding were items not easily produced by

any other technique, and included toys, boat fenders, display models and tanks needed in

special shapes and in small number. In recent years, the geometry of molded parts has

become even more complex as designers became familiar with the process and took

advantage of its potential. The products are flexible, both in terms of shape of the end

product and its size. For example, current product range from ear syringes to 100,000

liter storage tanks [1]. With the new development in the rotational molding technology,

the industry is pursuing more sophisticated products from dump-truck bodies to aircraft

ducts.
 6
1.6 The Advantages and Disadvantages of Rotational Molding

Compared with other processes like injection and blow molding, the rotational

molding process has its distinct advantages and disadvantages [1]. Some of the major

advantages offered by rotational molding are:

1. It can produce hollow parts which are virtually free from residual stress, have no weld

lines and have good thickness distribution and no waste scrap.

2. The costs for mold fabrication are low. Rotational molding is a low-pressure process

so that molds do not have to be high strength and can be produced with less time.

3. It can produce double-walled items, sandwich constructions and layered sections by

incorporating different colors or polymers.

4. Rotational molding leads itself to scaling up at relatively moderate cost. The process

is suited to produce very large parts.

5. Several molds of different sizes and shapes can be used simultaneously on the same

machine.

6. Metal inserts can be directly molded into parts.

Some of major disadvantages of rotational molding are:

1. Materials suited to rotational molding are more limited than for other processes.

2. Material costs are higher due to the cost of grinding pellets feedstock to a powder

form.

3. Labor is intensive as loading and unloading is primarily manual.

4. Cycle times are somewhat longer than other processes and thus it is not as economic

as injection or blow molding for large-scale production of small hollow parts.

 7
Although rotational molding is still considered as one of the simplest of the primary

plastics processing methods, it has made steady gains in sophistication over the past few

years. These advances include the advent of process simulation, use of C A D technology,

real-time process monitoring, pressurized molding, quick-change tooling, automated

mold-filling, and "ovenless" internally heated systems. With these new capabilities,

rotational molders are pursuing more ambitious applications.

1.7 Research Objectives and Thesis Outline

The objective of this work is to investigate the effects of different molding parameters

on the molding cycle in order to provide some guidelines for optimum molding cycle.

Further, this work focuses on the effects of powders on the densification process in

rotational molding. Characterization of the powder properties is performed and rotational

molding tests are conducted using a bench-scale machine.

This thesis is divided into five chapters. Chapter one simply introduces the rotational

molding process and development in the future. A review of previous studies relevant to

the rotational molding process and relevant to this study is presented in the second

chapter. Experimental equipment and procedure are presented in chapter three. The

experimental results and discussions are given in chapter four. The final chapter contains

the conclusions and recommendations for future work.

 8

CHAPTER TWO

LITERATURE REVIEW

Since the mid-eighties, a significant amount of research has shed considerable light

on the various aspects of rotational molding process. The Association of Rotational

molders (ARM) sponsors a variety of events as well as research and development

projects. More recently, The Society of Plastics Engineers (SPE) National Council

approved the formation of the Rotational Molding Division. A l l these activities largely

promote the development of rotational molding science and technology. The scientific

literature on the rotational molding process mainly covers the topics presented in the

following sections.

2.1 Simulation of Heat Transfer in Rotational Molding Process

Rao and Throne [3] were the first to give their attention to understanding and

simulating the melting process. With respect to the thermal/fluid considerations, they

proposed a two-layer powder flow model to describe heat transfer to the un-melted

plastic particles. Later, Throne [4-6] proposed an alternate heat transfer model, in which

the powder was assumed to be in static contact with the mold surface. The latter model

showed better agreement with experimental data. In 1982, Progelhof et al. [7] presented

an experimental study and model of powder densification and melting in rotational

molding. Crawford and coworker [8-15] proposed a numerical simulation for the heat

transfer in the rotational molding process. They commercialized the simulation software
 9
called ROTOSIM. ROTOSIM has the ability to predict temperature-time profiles and

molding cycle times. They thought that research into the heat transfer phenomenon might

be an essential step towards fully understanding the mechanisms of the rotational

molding process. In their models, modified boundary conditions for the solution of the

internal air temperature field were used. Bawiskar and White [16] followed Rao and

Throne's approach [3] and reached an analytical solution for heat transfer of the multi-

phase problem in rotational molding process. From the analytical solution, they

concluded that increasing (5 would have a more pronounced effect on reducing the cycle
m

time than increasing the oven setting temperature, here

fi = K A
O)
o C V

where p , C , V , and A are the density, heat capacity, volume and surface area of the
m m m

mold, respectively, and h is the heat transfer coefficient of the mold with air. This
m

finding somewhat challenges current belief on the heating cycle in rotational molding.

Gogos and coworkers [17, 18] have also presented a detailed analysis of the heat transfer

in the rotational molding process. They validated their model predictions by comparing

with experimental data presented by Nugent [9]. They showed that the oven temperature,

the polymer melting temperature, and the polymer to mold heat capacitance ratio were

key parameters affecting the melting time. Moreover, they demonstrated that a simple

lumped-parameter model could well predict the rotational molding process as a more

detailed differential model for a range of material properties and operating conditions that

is typical to the rotational molding of polyethylene resins.

 10
These researches have shed some light on the understanding of heat transfer

phenomenon in the rotational molding process, although it seems that all these models

have themselves limitations. Of course, due to the complexity of powder flow and the

transient nature of the process, further work in this field is needed to get a better insight

into the process.

2.2 Powder Sintering

Polymer sintering is of particular interest in rotational molding. It is viewed as the

fundamental and controlling mechanism for the process, because it commands a

significant part of heating time and has a profound influence on properties of the final

part. Resins with poor sintering behavior will either require longer heating time in the

molding cycle or result in the production of parts with large and numerous bubbles.

Powder sintering was first considered by Rao and Throne [3]. They broke the formation

of a homogeneous melt from powder particles into a two-step process. First, the powder

particles stick or fuse together at their points of contact, this fusion zone grows until the

mass becomes a porous three-dimensional network. They referred to this stage as

sintering. Second, at some point in the fusion process, the network begins to collapse into

the void spaces. These spaces are filled with molten polymer that is drawn into the region

by capillary forces. This step was referred to by Kuczynski [19] as densification.

A theoretical model to describe the early stages of viscous coalescence of two

spherical particles of glass was first derived by Frenkel [20]. More recently, Hopper [21-

23] developed an analytical model for the coalescence of two cylinders. Based on

experimental observations, Rosenzweig and Narkis [24, 25] proposed a geometrical

 11
model describing the polymer sintering. Moreover, they conducted an experimental study

with taking photographs of the sintering particles without interrupting the sintering

process. They found that the diameters of the sintering particles did not change

appreciably over a wide range of sintering process. Their experimental results had a good

agreement with Frenkel's model.

Van de Vorst [26, 27] performed a numerical analysis for a two-dimension viscous

sintering problem with non-smooth boundaries using a Finite Element Method. The

numerical solutions allowed for quantitative sensitivity analysis, i.e. the influence of a

perturbation of the initial diameter of the particles, the contact radius r and the neck

curvature on the shape and curvature of the region where those circles are touching.

These numerical results were found to be in good agreement with the analytical ones.

Bellehumeur et al. [28-31] studied polymer sintering extensively. They developed a

modified Frenkel's model for sintering. The model was based on the balance of the work

of surface tension and the viscous dissipation. A l l other forces, including gravity and

inertia force, are neglected. They proposed an analytical solution for the Newtonian

sintering process. The analytical results were found to be in good agreement with

experimental data.

It is generally known that resins with higher molecular weight and/or broad molecular

weight distribution are found to sinter at a lower rate. However, mechanical properties

and chemical resistance of molded parts increase with increasing the molecular weight

and the molecular weight distribution. It has also been shown that an increase in the

resin's elasticity is detrimental to the sintering process. Weber et. al. [32] compared the

processability of two resins with equivalent viscosities but different degrees of elasticity.
 12
Similar conclusions were drawn by Kontopoulou [33]. Recently, Guillen-Castellanos[34]

investigated the effects of molecular structure on the sintering of ethylene/a-olefin

copolymers. He found that increasing the comonomer content has a negative impact on

the sintering process.

2.3 Polymer Melt Densification and Bubble Removal

Considering the fact that rotational molding is virtually a shear stress and pressure

free process, viscosity is one of the most important parameters used to assess whether a

resin is suitable for this process. The presence of bubbles in the molded part is a serious

problem, because it can affect the mechanical properties of the parts. Moreover, the

presence of bubbles and pitholes (bubbles on the outer surface of the part, which is

adjacent to the mold) poses a problem to the part appearance and aesthetics.

In an initial attempt to describe the bubble formation problem relevant to rotational

molding, Rao and Throne [3] drew extensively from the theories of metal sintering and

densification. They had noted that extensive porosity existed on the surface of the part in

contact with the mold. After analyzing the forces acting on a spherical bubble growing on

the mold surface, they concluded that the formation of voids is intrinsic to the rotational

molding of plastic powder. The voids could not be released from the mold surface, since

for most cases the buoyant force is insufficient to overcome the surface tension force.

Later, Progelhof et al. [7] used a flat plate simulator to observe the densification process.

The most striking phenomenon they observed was the slow movement of the bubbles to

the free surface. They also observed that the bubbles showed signs of coalescence. In

their experiments, however, they used polymer in pellet forms rather than powder. As a
 13
result, the sizes of bubbles formed in Progelhof s experiments were significantly larger

than that typically seen in the densification process of polymer melt.

Kelly [35] utilized a variety of optical microscope techniques to study the formation

and disappearance of bubbles during the densification of polymer powder. Based on his

observations, he concluded that the bubbles did not migrate in the melt but simply shrink

sizes and disappear finally as the air dissolves in the polymer. He also mentioned that

there appeared to be a critical minimum and maximum bubble diameters. Bubbles

smaller than the critical minimum diameter will disappear rapidly and bubbles greater

than the maximum size will not dissipate regardless of temperature or heating time

because the surface tension of bubbles could not generate high enough pressures inside

the bubbles to help dissolve the gases. Crawford and Scott [36] presented a detailed study

of the phenomena occurring during the formation and removal of bubbles. They

confirmed Kelly's suggestion that bubbles remain virtually stationary in the melt. X u and

Crawford [37, 38] presented an empirical formula for the bubble dissolution. The

parameters in the formula were regressed from the experimental data. Spence and

Crawford [2, 39, 40] published extensive studies on the process variables affecting the

formation and removal of bubbles in rotational molding. They found that low viscosity

materials produced products with no bubbles or pitholes when rotationally molded. They

also found that molded parts near "hot spot" of the mold surface contained no bubbles.

In 1999, Gogos [41] published an analytical solution for bubble removal in rotational

molding. He neglected the viscous effects on the shrinkage phenomena. From the

calculating results, he concluded that surface tension contributed substantially to the

concentration gradient that drives bubble shrinkage. At a vanishingly small degree of

 14
saturation, the bubble lifetime was very short, and the effect of surface tension was

negligible. He also explained that a pressure increase imposed on a saturated polymer

melt could lead to a steep concentration gradient in the vicinity of the bubble/melt

interface and lead to fast bubble shrinkage. Kontopoulou et al. [42] presented a

theoretical model which included the effects of viscous forces. Numerical method was

adopted to solve the model. From the result, they concluded that bubble dissolution

depended significantly on initial bubble size, surface tension and air concentration in the

polymer melt, but it was not influenced considerably by melt viscosity. They also

claimed that the bubble content initially presented in the polymer melt was the most

important factor governing the bubble dissolution. Their results are, otherwise, consistent

with those presented by Gogos [41]. Tiang and Bellehumeur [43] recently also developed

a numerical method to simulate bubble formation and dissolution in rotational molding.

They used different configurations to simulate bubble formation and dissolution and

successfully combined models of heat transfer, powder sintering, and bubble formation

and dissolution into their simulation model. With this numerical method, they evaluated

the effects of molding conditions on the densification phenomenon in the rotational

molding process.

2.4 Effect of Powder Properties on the Rotational Molding Process and Properties of

Molded Parts

Qualitatively, much has been written about the types of powder suitable for rotational

molding. Rao and Throne [3] suggested that powder particles with a shape similar to that

of a rounded cube would favor heat transfer while a spherical shape would lead to the
 15
best flow characteristics. Particles with 'tail' would cause bridging effect and trap high

level of bubbles.

Powders are mainly produced from the grinding of plastic pellets. McDaid and

Crawford [44] investigated grinding process to improve powder quality. They found that

powder quality was very dependent on processing temperature and rate of cooling after

grinding. They showed that the dry flow and bulk density values improved dramatically

as the processing temperature increased. Heating powder at temperatures below melting

point could also improve powder quality. Improved powder quality helped to reduce

surface porosity and internal voids.

Particle size distribution is an important index of powder rotational moldability and

has significant effects on the properties of molded parts and process economy. Rao and

Throne [3] mentioned that the smaller the powder size the better the heat transfers. The

limitations for the particle sizes were that, first, grinding of powder less than 100 mesh

would lead to excessive material losses and high cost of grinding and, second, tumbling

of very fine powders within a mold would build up high static charges which aid in

agglomerating the powders. Molded parts with small particle sizes would lead to an

uneven melting and non-uniformity of part wall thickness. A single criterion has not been

defined to assess whether a given powder would be rotationally moldable or not. Usually,

rotational molders would consider the particle size distribution as well as measurements

of the bulk density and flow ability.

Crawford [45] also presented a qualitative relationship of particle size and properties

of the molded parts and molding process as in Figure 2.

 16

tu
Q.
2
CL

Paride size

Figure 2. Effect of Particle Size on Properties

The main effect of powder shape and particle size distribution is on the flow ability of

the powder. On the other hand, the powder flow in the heated mold environment might be

different from ambient conditions due to deformation or coalescence of the powders.

Throne [46] recently presented an article about the powder flow during rotational

molding. Understanding the rheological forces acting on the powder bed at elevated

temperature might help pinpoint potential process problems.

2.5 Effects of Additives on the Rotational Molding Process and Properties of Molded

Parts

Rotationally molded parts are often pigmented for aesthetics or for protection against

other elements attacking or light degradation. Pigment can be added by melt

compounding and grinding or simply by dry blending with the polyethylene powder.

Melt compounding is more expensive but gives a better color intensity and better

physical properties. Pigments added by dry blending are usually not uniformly distributed

in the molded part but tend to concentrate near the mold surface.
 17
Crawford et al. [47] studied different colors and different kinds of pigments. They

concluded that pigmentation levels should generally be lower than those currently used

because lower pigmentation could maintain both good color and significantly better

toughness. Parts with organic pigments showed poorer impact properties than inorganic

pigments. Muller [48] worked on carbon black and U V absorbers and found that the loss

of impact strength was much more severe in dry blend materials than in compounded

materials and all combinations of blacks and U V absorbers reduced the impact properties

drastically. DeFranco [49] explored producing color parts using liquid color pigments.

With the typical pigmentation levels used in rotational molding, liquid color agents

increased color strength and opacity of molded part. A n unexpected advantage with the

liquid color product was that coated powder was static-free after treatment, making

subsequent handling easier.

In order to improve the stiffness of the rotationally molded parts, Wisley [50] used

glass fibre to reinforce the molded parts. No improvements in mechanical properties were

obtained with dry blending polymer and glass fibres. However, with maleic anhydride as

a coupling agent to produce glass fibre reinforced polymer pellets, compared with virgin

polyethylene, the tensile strength and flexural modulus of molded parts increased by 54%

and 127% respectively. Chaudhary et al. [51] investigated the effect of processing

enhancers. They found that blending small amounts of low molecular weight additives

with polyethylene promoted particle coalescence and bubble removal during rotational

molding, resulting in shorter cycle times without adversely affecting impact strength.

Spence [52] found the same result with additives such as stearamide.
 18
Murphy et al. [53] studied the addition of silicate clays in polyethylene. They

investigated two kinds of clays and found that polyethylene had a marked improvement

in storage moduli when organoclay was added. Slightly higher crystallinity values were

recorded for the resins with organoclays and increases in viscosity depended on the kinds

of clays used.

2.6 New Processes and New Products of Rotational Molding

Crawford and coworkers [54, 55] analyzed the effects of cooling during rotational

molding. They investigated the mold with sealing and with internal cooling. They found

that sealing mold helped reduce shrinkage and internal mold cooling caused an increasing

cooling rate of the plastic part and thus reduced the cycle time. They also found that

internal cooling caused a reduction of shrinkage of the molded part. Spence [56]

commented on the effects of mold pressurization on the molded part properties. After all

the powders in the mold were melted, a positive pressure was applied. This procedure

was found to help remove bubbles from the polymer melt and reduce the molding cycle

time and part shrinkage. Chen et al. [57], on the other hand, concluded that pressurized

mold had little or no effect on the mechanical behavior of the molded parts and the

primary role of mold pressurization was simply to hold the solidified polymer against the

mold wall, thus reducing warpage and shrinkage. They commented that mold

pressurization helps reducing the total molding cycle time. Evans [58] investigated

rotational molding under vacuum conditions. He found that under vacuum conditions

tougher molded parts were obtained with reduced cure times. He also found that bubble

dissolution rate under vacuum conditions was faster than that under normal conditions.
 19
He explained his result according to the "boiling" effect, that is, the low end or "light"

chains or monomers vaporized into this vacuum void.

Harkin-Jones and Crawford [59-61] studied rotational molding of liquid polymers.

Liquid polymers offer a number of advantages over powder to the rotational molders.

With many liquid polymers, heating and cooling of the mold may not be required and

severe thermal cycling of the mold tools may be avoided. The total molding cycle time

can be as short as two minutes for some materials. In some cases, exothermic heats of

reaction may be used to heat the mold and the processing of certain liquid polymers is

very energy efficient. There are, however, a number of problems which are inherent to

the processing of liquids. These problems include the difficulty in controlling reaction

viscosity, uneven material distribution and bubble formation due to the movement of

material pool during molding cycle. They concluded that the optimization of the ratio of

retarder to catalyst and temperature control of the mold is key to successfully molding

liquid polymers.

Liu et al [62,63] studied rotational foam molding of polyethylene and polypropylene.

They concluded that to get a large cell population density and uniformly distributed cells,

the polymer and chemical blowing agent should be well mixed initially. Takacs et al. [64]

published an article about foaming with microspheres in rotational molding. They used

hollow microspheres with thermoplastic shells encapsulating gas as a foaming agent and

successfully obtained foam with fine cells and smooth surface.

Wisley [65] described the method of producing multiple layer rotational products. A

drop box was used to store the second charge of material. The drop box was insulated to

prevent the material from melting prematurely. With the help of Rotolog [66], they could
 20
know precisely at what temperature the second polymer was introduced into the mold.

With the multiple layers of rotationally molded products, the best combination of

properties, processibility, and cost can be obtained. Pop-Iliev et al. [67] studied single

step rotational foam molding of skin-surround polyethylene foams. Using single-step

operation significantly improved the efficiency of the molding process and the structural

homogeneity of molded products. However, the main problem with single-step operation

was that it must be guaranteed that the non-foamable thermoplastic resins first totally

stick on the mold surface prior to the activation of the forming resin.

Teoh et al [68,69] published research results on computer controlled rotational

molding of medical prostheses. Advances in computer control enhanced the versatility of

the rotational molding process, enabling an examination of the effects of varying rotation

speeds, speed ratio as well as rotation modes.

 21
CHAPTER THREE

EXPERIMENTAL

3.1 Rotational Molding Experiments

The molding experiments were conducted using a uni-axial bench-scale machine. The

rotational molding machine consists of the oven, mold, fans, rotating shaft, motor,

thermocouples, controller and computer data gaining system. Since the shaft-end of the

mold, which is connected to a motor, remains in a stationary axial position, the oven with

inner diameter 300 mm and length 385 mm is placed on four rollers so that it can slide

along the support table. Two electrical, semi-circular heating panels are responsible for

heating the oven to a temperature within the range of ambient temperature to 600°C. To

ensure proper circulation of the heat and uniform oven temperature distribution, two fans

are placed in the front of the oven. The front window is equipped with a glass window.

The mold used in the experiment is a steel cylinder with a polished inner surface and a

black painted outer surface. The cylinder inner diameter is 101 mm and the length is 154

mm. The front and back plates covering the cylinder have a diameter of 144 mm. The

plate opposite to the shaft side is also equipped with a glass window (110 mm in

diameter). The rotation speed of the mold can be adjusted through the control panel. For

the purpose of comparison, the rotating speed of the shaft was set at 5 rpm. Once the

oven is placed over the mold, the two windows (oven and mold cover) are aligned,

allowing visual observation of the powder flow within the mold.

There are four thermocouples used to monitor the temperatures at four different

locations. Thermocouple 1 is used for the oven temperature control and is placed at the
 22
middle and the top of the oven 20 mm to the oven inner wall. Thermocouple 2 is placed

in the back of the oven and 150 mm to the inner surface of the back cover and 40 mm to

the oven inner wall. Thermocouple 3 is placed through the shaft and into the inside of the

mold (150 mm to the front edge of the oven) to measure the inside air temperature. Lastly

thermocouple 4 is placed as a safety measurement 150 mm to the front cover inner

surface and 40 mm to the oven wall to make sure that the oven does not overheat. FP-TC-

20 FieldPoint (National Instruments) was used as an on-line temperature data acquisition

device. FP-TC-20 is connected to the computer by a cable, so that the temperature

changes can be displayed on the computer's screen.

The oven is heated by electricity and controlled by Watlow's series 93 controller.

Series 93 controller features include dual output. The primary output can be heating or

cooling while the secondary output can be a control output opposite the primary output.

Both outputs can be selected as either PID or on/off. PID settings include proportional

band, reset/integral, and rate/derivative. Due to the constant oven temperatures used in

the experiments, only the proportional band (pb values) setting is selected. The uni-axial

rotational machine and control panel are illustrated in Figure 3.

Good control of the oven temperature is crucial for the accuracy and repeatability of

the experiments during molding tests. The parameters of the oven controller were tuned

up to minimize the variations in the oven temperature. The relationships between

proportional band settings (pbl) of the controller and oven temperature profiles were

examined (Appendix Figure 21). For the purpose of quick response to the oven

temperature changes, small pbl values are preferred and the proportional band setting

(pbl) of 3 was selected.

 Control panel

Figure 3 Bench Scale Rotational Molding Machine

 24
With mold in the oven, the spatial variation in the oven temperature is within ± 3.2°C

(95% confidence) (See Appendix Figure 22).

3.2 Material Properties

Experiments were conducted using a commercially ground polyethylene resins. One

linear low density polyethylene resin TR.0242 was used in this work, which was supplied

in powder form by N O V A Chemicals Corporation. The properties of the resin were

provided by the resin manufacturer and are given in Table 1.

Table 1. The Properties of Rotational Molding Material

Resin TR0242

Melt Index (g/10 min) (ASTM D792) 1.8

Density (g/cm ) ( A S T M D1238)

3
0.942

Flexural Modulus (MPa) (ASTM D790) 970

Tensile Strength (MPa) (ASTM D638) 22.3

3.17 mm 60
A R M Low Temperature
Impact Strength (ft.lbs)
6.35 mm 180
Large parts,
End-use Applications
Storage tanks

3.3 Powder Characterization

A set of sieves vertically stacked on a vibrating unit is used to determine the particle size

distribution. 50g of powder is used for measurement. Seven sieves are mounted vertically

in descending order of mesh sizes: 35, 40, 50, 60, 70, 80, 100. These are, in microns, 500,
 25
425, 300, 250, 212, 180, and 150. The weight found in each pan after 10 minutes sieving

gives the percentage mass of each band of particle size. The particle size distributions for

the resins used in the experiments are shown in Figure 4.

3.4 Molded Part Characterization

3.4.1 Thickness Measurement of Molded Parts

The thickness distribution was determined for each molded part. A ruler and a caliper

were used to measure the thickness for every 0.5 cm interval along the axis of the

cylinder, starting from the shaft end towards the window. A n average of two values is

used as the thickness value for each point. The cutting scheme of the molded parts for

characterization is illustrated in Figure 5.

3.4.2 Density Measurement of Molded Parts

Electronic Densimeter MD-200s is used for density measurements. Electronic

Densimeter MD-200s adopts Archimedes' principle and the determination of relative

density values is based on the density of water at 4°C as a reference. Liquids other than

water can also be used provided that their density is known and that they are not

corrosive or dissolve to the materials of water tank, basket and steel angle. First, the

sample is weighted in the air. Then the buoyancy forces (water displacement) are

measured by entrapping the sample between the water surface and the metallic angle. The

angle is used to ensure that samples get submerged into the water since the density of

plastic is less than that of water. The factors that affect the test results are the possible

vibration of the table on which the densimeter is installed, bubbles attached on the sample
50.0

40.0
TR0242
30.0

20.0

10.0

0.0 i I • •
>35 35-40 40-50 50-60 60-70 70-80 80-100 <100
Size interval ( m e s h )

Figure 4 Particle Size Distribution of Experimental

Material
 27
surface and the presence of water drops on the basket during the second stage of the

operation.

3.4.3 Bubble Size Distribution

The bubble number and bubble size distribution were obtained from determining

bubble numbers and sizes on a thin plastic strip, which was cut from the molded sample

(see Figure 5 for reference). Totally 6 strips taken from different locations were analyzed

for each molded part. The thin strip was fixed onto a glass slide and magnified pictures

were taken one by one until all the strip area was photographed (total 13 pictures were

obtained for each strip) by using a C C D camera connected to an Olympus optical

microscope. Image analysis was performed on the pictures using ImagePro software,

recording the sizes as well as the locations of the bubbles detected within the plastic

stripes.

3.5 Experimental Procedure

Experiments are carried out on a uni-axial bench scale rotational molding machine.

The main advantages of using the uni-axial bench scale machine are that the inside mold

temperature can be easily monitored and the flow of powder inside the mold can be

visualized. The oven is preheated to the preset temperature when the molding powder is

prepared and loaded into the mold. The oven temperature shows a drastic drop during the

operation of opening the oven and moving the oven covering the mold. To compensate

for this drop and to ensure a rapid stabilization of the oven temperature during a molding

experiment, the oven preset temperature is initially set at a higher value than that for the
 28

Cut lines

Sample six pieces Sample strip for

cutting scheme bubble count

Cutting Line

Sample piece for Sample pieces for

thickness measurement density measurement
 29
molding experiment and it is adjusted after the insertion of the mold into the oven. For

different experimental oven temperatures the preset temperatures for the preheating have

been determined by trial and error (Table 2). The shot weight of powder used in all test

was set to 100 g.

Table 2. Oven temperatures and corresponding preset temperatures

Required Oven Temperature (°C) 250 350 425

Preset Temperature (°C) 330 480 590

Once the powder is loaded into the mold and the oven temperature has reached the

preset value, mount the mold on the shaft and adjust the rotating speed of the shaft to 5

rpm. After that, start the Fplogger program (data acquisition) and set the data-recording

time interval to 10 seconds. At this time, the data acquisition system is ready to record the

data. The preset temperature is reduced to the selected experimental oven temperature as

soon as the oven is pulled over the mold. Air temperature inside the mold then increases

gradually. The powder flow inside the mold can be observed through the two glass

windows (oven and mold). It is generally observed that some powder first sticks on the

middle part of the mold and then the powder sticks on the other part of mold. As the

temperature continues to increase, the powder melts. The heating cycle of the molding is

determined by the time required for the air inside the mold to reach a value within 196-

200°C. For polyethylene, this range of temperatures has been found to be advantage in

ensuring bubble dissolution in the melt while avoiding degradation of the material.

Normally the oven is pulled away from the mold at temperature slightly lower than that

interval. At that point, the mold temperature is still higher than that of the polymer and

the air inside the mold. Heat continues to be transferred from the mold to the polymer and
 30
the air inside the mold and the temperature of the air inside the mold continues to

increase. After a few trial-and error tests, for different oven temperatures, the inner air

temperatures at which the mold should be moved out of the oven in order to get the

maximum inside mold air temperature within the range of 196-200°C are listed in Table3

Table 3 Oven temperatures and corresponding removal temperatures

Oven temperature (°C) 250 350 425

Removal temperature (°C) 197-198 172-174 132-134

When the temperature of air inside the mold reaches the removal temperature, the

mold is moved out of the oven and the cooling fan is immediately turned on. When the

temperature reaches the easy handling temperature (normally 50°C), the whole molding

cycle ends and the recording is stopped. The mold is taken off from the shaft and opened.

The molded part is removed from the mold and labeled for property characterizations.
 31
CHAPTER FOUR

RESULTS AND DISCUSSIONS

4.1 Effect of Mold Characteristics on the Molding Cycle

The outside surface of the mold was painted with high temperature black paint.

Figure 6 compares the molding cycles with the painted mold and unpainted mold

(metallic surface). The molding cycle is much shorter when the black painted mold is

used especially at high oven temperature. It is easy to understand that the black painted

mold absorbs more heat than the unpainted mold due to heat absorption from radiation

directly proportional to the gray degree of the surface. Furthermore, the energy of

radiation is proportional to the 4 power of the temperature of the heating source.

th

Therefore, at the present conditions of forced air convection, the mold heating is a result

of combination of radiation and convection. From this result, it is recommended that

making the mold surface black is one way to improve the heating efficiency and reduce

the molding cycle for rotational molding applications.

4.2 Description of the Molding Cycle

Rotational molding cycle has previously described by other researchers Crawford [1]

and Nugent [9]. As a principle step toward to understanding rotational molding process,

molding cycle again presented here. As indicated in Figures 7, 8 and 9, the molding cycle

starts at point A , when the mold containing powder particles is inserted into the oven

cavity. During the induction phase (AB region on the figures), the powder is tumbling
250

O1 ! 1 1 1 1 1 !

0 5 10 15 20 25 30 35 40

Time (min)

Figure 6 Effect of mold color on molding cycle time

(oven temperature 350°C, 100g, 5rpm, particle size: 40-50mesh)
O -] ! , , , , , ,
O 5 10 15 20 25 30 35 40
Time (min)

Figure 7 Molding Cycle and O v e n T e m p e r a t u r e (TR0242,

Ove n T e m pe rature 250°C,100g, 40-50mesh, No. 020221 AB)
500
450
400
350
300
Thermocouple 1 (control)
250 Thermocouple 2 (Back)
Thermocouple 3 (air inside mold
200 Thermocouple 4 (safety)

150
100
50
0
10 15 20 25 30

Time (min)

Figure 8 Molding Cycle and Oven Temperature (TR0242, Oven

Temperature 350°C,100g, 40-50 mesh, No. 020221BB)
 600

500
O
^ 400 11 * * * *-i i i * *
o
Thermocouple 1 (control)
re 300 Thermocouple 2 (Back)
Thermocouple 3 (air inside mold
Thermocouple 4 (safety)

10 15 20 25

Time (min)

Figure 9 Molding Cycle and Oven Temperature (TR0242, Oven

Temperature 425°C,100g, 40-50 mesh, No. 020221CB)
 36
about inside the mold but the temperature of the internal surface of the mold is below that

at which powder particles start to stick on the mold surface. At point B, the powder starts

to stick to and melt on the mold surface. As the polymeric material melts, much of the

thermal energy added to the system (mold, polymer, air) is used to change the phase from

solid to melt. This explains why the increase rate of air temperature inside mold is lower

for region B C than that of regions A B and CD. At point C, however, all the powder has

melted and there is a coating of melt on the inside surface of the mold. The heat input is

therefore directed back to heating the mold, the polymer and the air inside the mold.

When the mold is removed from the oven and cooled by the forced air, the internal air

temperature does not drop immediately but continues to rise for a short period of time.

The temperature jumps in this interval depend on the oven temperatures. The higher the

oven temperature, the larger the temperature jumps. After reaching the point D, the

temperature starts to drop due to forced air-cooling. At point E the solidification of the

polymer is taking place and some thermal energy is released. At Point F, solidification of

the melt is completed. At point G, the mold has reduced its temperature low enough to be

handled manually and the part can be removed.

4.3 Effect of Oven Temperature on the Molding Cycle

It is seen that oven temperatures have significant effects on the molding cycle when

comparing the curves presented in Figures 7 to 9. With the same maximum temperature

of the air inside the mold, for the oven temperatures of 250°C, 350°C, and 425°C, the

corresponding heating time of molding cycle is 16 min, 8 min and 5 min, respectively. In
 37
the real production, the heating stage has a high impact on the productivity due to the

oven occupation. Therefore, productivity will be improved with higher oven temperature.

4.4 Molded Part Properties

4.4.1 Thickness Distribution

The thickness distributions of the molded parts for different oven temperatures are

plotted in Figures 10 and 11. The general trend is that in the direction from the shaft end

of the mold towards the window the thickness steadily increases until mid-section and

decreases once it is near the section by the glass window.

It is unlikely that polymer melt flow has an effect on the thickness distribution due to

very high viscosity of the polymer melt. The thickness distribution of the molded part is

probably mostly affected by the inside surface temperature distribution of the mold. In

our experiments, it was generally observed that more powder accumulates in the middle

section of the mold. One possible reason for this is that the middle part of the mold might

receive more radiation energy than the end sections because the absorption surface is

coaxial to heat generation surface. Furthermore, the mass of metal heated in the end

sections is larger than that in the middle section. We speculate that when the mold is put

in the oven, the temperature of the middle section of the mold increases at a faster rate

than that of the shaft and window sections. Therefore, the powder first sticks on the

middle section and some powder becomes melted while the other part of the mold surface

is still empty. As the tumbling continues, more powder will stick on the melted powder in

the middle section. That is likely the main reason for the uneven thickness distribution.
O 0.2 0.4 0.6 0.8 1
Relative distance to shaft

• 020221AB(oven temperature 250°C)

020221BB(oven temperature 350°C)
- - A - - 020221CB(oven temperature 425°C)

Figure 10 Thickness Profiles in the Molded Parts (Along the

Longitudinal Axis) (TR0242,100g, 40-50mesh, 5rpm)
2.90

1.50 4 1 1 1 1 1
0 0.2 0.4 0.6 0.8 1
Relative distance to shaft

-• 020305AB (oven temperature 250°C)

020305BB(oven temperature 350°C)
A- - 020305CB(oven temperature 425°C)

Figure 11 T h i c k n e s s Profile in the Molded Part (Along the Longtitudinal

Axis) (TR0242,100g, P o w d e r as Received, 5rpm)
 40
4.4.2 Density of the Molded Parts

MD-200s densimeter is used for the density measurement. Basically, because the

MD-200s densimeter uses the Archimedes' principle to measure the density, the sample

needs to be weighted two times, one time for the weight in the air and one time for the

volume (weight in the water), with a ±0.01 g accuracy. If the average density of molded

part is assumed to be 0.925, then, the volume for each piece when cutting the sample to 12

equal pieces (4 pieces along 0 direction and 3 pieces along the axial direction) equals to

V=l00g (shot weight)/0.925 (density)/12(piece)=9cm 3

(2)

The accuracy for density measurement equals to

ÔD 3D
AD = ± AW + AV = ±0.0015g/cm 3
(3)
dW dv
where D, W and V are density, weight and volume of each piece, respectively. For other

cutting schemes, the results are given in Table 4 and it shows that the absolute error of

density measurement increases as the cutting number increases. A more accurate result is

obtained with a larger volume sample for the density measurements. Smaller pieces may

provide some information about the variability in the density across the molded part,

which would be relevant for parts molded using a mold with a cross section shape

different than that of a cylinder.

Table 4. Absolute error on the density measurements

Number of pieces cut Approximated volume Absolute error for density
from the molded part of each piece (cm ) 3
measurement (g/cm ) 3

12 9.0 ±0.0015
24 4.5 ±0.0030
36 3.0 ±0.0045

48 2.25 ±0.0061
 41

The results for repeatability of density measurement are presented in Appendix (Table

5 and Table 6). Figure 12 presents the density of different section of molded parts

produced at 3 different oven temperatures. The sections near the shaft and near the

window have a lower density compared to the rest of the mold. Higher density values in

the molded part are obtained from the sections located in the middle of the mold. This

trend can also be explained based on a heat transfer analysis of the molding cycle. During

the molding cycle, the middle section of the mold may be heated at a faster rate than the

end section as discussed in section 4.4.1. It is estimated that the polymer melt in the

middle section remains at higher temperature for a longer period of time, which would

favor a better densification, particularly the bubble dissolution process, compared to the

end sections of the mold.

The density profiles obtained for the three different oven temperatures show similar

trends. The variations in the density with the axial position in the mold are, however,

more pronounced at high oven temperature. Small variations in the molding heating time,

while maintaining constant oven temperature, also have important effects on the density

profiles, as shown in Figure 13 to 15. These differences in heating time are not very large

but they have repercussions on the maximum temperatures reached within the polymer

melt which in turn affect the densification process. Since the heating time, and thus the

maximum air temperature reached in the mold, has a strong effect on the molded part

density, particular attention should be paid to this aspect of the molding conditions when

investigating other effects on the densification process.

0.94

Relative distance to shaft

••—020221 A B (oven temperature. 250°C)

« — 020221BB (ove n te m pe rature .350°C)
•A—020221CB (oven t e m p e r a t u r e . 4 2 5 ° C )

Figure 12 Density Profile of Molded Part

(TR0242,100g, 40-50mesh) (4 Parts Average for Each Point)
 43

- • — 020211BB,maximum inside air temperature 200.1 °C

- • — 020220BB, maximum inside air temperature 199.4°C
-A— 020315BB, maximum inside air temperature 197.8°C

0.2 0.4 0.6 0.8

Relative distance to shaft

Figure 13 (a) Density Profile in the Molded Parts (4 Parts Average)

(TR0242, 100g, Oven Temperature 350°C, Powder as Received)

100 J 1 1 1 1 1 1 1 1 1
4 5 6 7 8 9 10 11 12 13
Time (min)

Figure 13(b) Molding Cycle for Different Maximum Inside Air Temperatures
(TR0242, 100g, Oven Temperature 350°C, P o w d e r as Received)
 44

0.94 !

0.935

0.91 I r— ! 1 1
0 0.2 0.4 0.6 0.8 1
Relative distance to shaft

-•— 020207AB, maximum inside air temperature 201.8°C

• — 020207BB, maximum inside air temperature 196.1°C
-X-—020315CB, maximum inside air temperature 198.0°

Figure 14(a) Density Profile in the Molding Parts (4 Parts Average)

(TR0242,100g, Oven Temperature 425°C, Powder as Received)

Figure 14(b) Molding Cycle for Different Maximum Inside Air Temperature
(TR0242,100g, Oven Temperature 425°C, Powder as Received)
 45
0.926 - , —
0.925
^ 0.924
g 0.923
-H 0.922
O)
~ 0.921
•- 0.92
(A

« 0.919
° 0.918
0.917
0.916
0 0.2 0.4 0.6 0.8 1

Relative distance to shaft

Figure 15(a) Effect of Particle Size on Molded Part Density
(TR0242,100g, oven temperature 250°C)

« — 0 2 0 3 1 9 A B , maximum inside air temperature 199.8°C,40-50mesh

•àc—020315AB, maximum inside air temperature 199.0°C, Powder as received
• • — 020326CB, maximum inside air temperature 199°C, <70mesh

Time (min)

Figure 15(b) Effect of Particle Size on Molding Cycle (TR0242,

100g, Oven Temperature 250°C)
 46
The effect of particle size on the density is shown in Figure 15. It is illustrated that the

part molded with larger particle size (40-50 mesh equivalent to 420-297 micron) has a

higher density than that of the parts with small particle size. This may be due to

differences in the powder packing arrangement leading to the formation of bubbles with

different size distribution. It can also be due to a difference in static built-up, often caused

by the presence of fine powder particles.

4.5 Bubble Size and Bubble Distribution

The formation of bubbles in the melt during powder melting and densification is

almost unavoidable. The bulk density of powder is typically 30% to 40% that of the

polymer. During the melt deposition process, pockets of air get trapped into the melt and

form bubbles. Due to the high viscosity of the material and the small size of the bubbles

they remain essentially stationary. Experimental and theoretical analysis of the process

have shown that the parameters affecting the initial size of the bubbles formed are as

follows [2,35,38,41,72]:

• the powder characteristics such as particle size, particle size distribution, shape,

packing density,

• the melting deposition rate which is controlled by the oven temperature, mold

• characteristics and polymer thermal properties,

• the polymer rheological properties (viscosity, elasticity) and surface tension.

While parameters affecting the rate of dissolution of the bubbles are as follows:

• the degree of saturation in the melt which is affected by the pressure, temperature,

and density of bubbles dissolution into the melt,

 47
• the melt temperature which also affects the gas dissolution into the melt,

• the initial size of the bubble,

• the polymer viscosity and interfacial tension.

Variations in the bubble size and size distribution with respect to axial position along

the length of the mold were observed. Higher number and larger bubbles are seen at

positions close to the shaft and close to the window. The results presented in this thesis

were obtained from the analysis of mid-section of the mold where heat transfer is

assumed to be unidirectional. Figure 16 gives an example of bubble distribution across

the plastic thickness of a molded part. Figures 17 and 18 present some preliminary results

on the effect of molding conditions on the number of bubbles and bubble size distribution

in molded part. It can be seen that as the oven temperature increases the number of

bubbles present in the melt decreases. The results in Figure 19 indicate that the bubble

size distribution slightly changes with increasing the oven temperature. We speculate that

both the oven temperature and the heating time affect the process of bubble formation

and dissolution. A n explanation for the results presented in Figure 17 and 18 can be

formulated based on a theoretical analysis of the densification process. Comparing to

high oven temperature, at low oven temperature the melt deposition proceeds over a long

period of time and on average the temperature of the melt is low.

Bellehumeur and Tiang [72] have presented an analysis of the heat transfer and

densification process in rotational molding. They showed that low oven temperatures

result in a slow melt deposition process which in turn leads to the formation of slightly

smaller bubbles but low melt temperature leads to significantly slower bubble dissolution

rates. The heating time at low temperature needs to be longer to allow for complete
 Free Surface

Molding conditions: Resin TR0242, Oven Temperature 250°C, shot weight 100g, Particle size: As received, rotating speed:
5rpm, maximum temperature of air inside mold: 200.4°C, Sample position: 7.5-8.5 cm to shaft side, Magnification 12.5X,
Sample No. 020411 A B .

Figure 16 Optical Micrograph of a Thin Cross Section of a Molded Part

00
O J 1 1 1 1 1 1 1
0.4 0.45 0.5 0.55 0.6 0.65 0.7 0.75
Relative distance from shaft

-•—oven temperature 250°C, maximum inside air temperature 200°C

-•—oven temperature 350°C, maximum inside air temperature 200°C
-ù—oven temperature 425°C, maximum inside air temperature 197°C

Figure 17 The Effect of Oven Temperature on the Number of

Bubbles (TR0242, Shot Weight: 100g, Powder as Received, 5-
sample Average, Plastic Area Analyzed: 800 mm )2
0.45
0.4
0.35
0.3
0.25
0.2
0.15
0.1
0.05
0
0.01-0.12 0.12-0.15 0.15-0.25 0.25-0.35 0.35-0.5 0.5-0
B u b b l e s i z e interval ( m m )

No. 0 2 0 5 2 9 A B . m a x i m u m i n s i d e air t e m p e r a t u r e 200°C

No. 020529BB, m a x i m u m i n s i d e air t e m p e r a t u r e 197.4°C
No. 020529CB, m a x i m u m i n s i d e air t e m p e r a t u r e 196.5°C

F i g u r e 18 B u b b l e Size D i s t r i b u t i o n in the M o l d e d Part (TR0242, S h o t

W e i g h t 100g, O v e n T e m p e r a t u r e 4 2 5 ° C , P o w d e r a s R e c e i v e d ,
M i d d l e S e c t i o n , A n a l y z e d A r e a : -800 m m )
2
 1.4
¡ 1.2

0.01-0.12 0.12-0.15 0.15-0.25 0.25-0.35 0.35-0.5 0.5-0.7

Bubble s i z e interval (mm)

—No.020326CB, oven temperature 250°C, maximum inside air temperature 199°C

« — N o . 020518AB, o v e n temperature 350°C, maximum inside air temperature 196.2°C
— N o . 020518BB, o v e n temperature 425°C, maximum inside air temperature 196.3°C

Figure 19 Bubble Size Distribution in the Molded Parts (TR0242, Shot Weight
100g, Particle Size <70mesh, Middle Section, Analyzed A r e a -800 m m )
2
 1.2

0.01-0.12 0.12-0.15 0.15-0.25 0.25-0.35 0.35-0.5 0.5-0.7

Bubble s i z e interval ( m m )

•4— No. 020518BB,maximum i n s i d e air t e m p e r a t u r e 1 9 7 ° C . p o w d e r < 7 0 m e s h

• No. 020529BB, m a x i m u m i n s i d e air t e m p e r a t u r e 1 9 9 ° C , p o w d e r as r e v e i v e d
No. 020319CB,maximurn i n s i d e air t e m p e r a t u r e 1 9 9 ° C , 4 0 - 5 0 m e s h

Figure 20 T h e Effect of Particle S i z e o n B u b b l e S i z e Distribution

in the M o l d e d Parts (TR0242, s h o t w e i g h t 100g, o v e n
t e m p e r a t u r e 4 2 5 ° C , m i d d l e s e c t i o n , a n a l y z e d a r e a ~800 m m )
2
 53
dissolution of bubbles. In contrast, a high oven temperature leads to rapid melt deposition

and fast bubble dissolution rates. At high oven temperature, however the heating cycles

are usually very short to avoid possible thermal degradation of the polymer and as a

result the bubbles do not always have enough time to completely dissolve into the melt.

For the sample with oven temperature 425°C, although the molding cycle is much shorter

compared to samples with oven temperature 250 and 350°C, the samples considered in

this work fewer bubbles. The low bubble content seen in the part molded at 425°C seems

to indicate that temperature dominated the densification process rather than the time

allocated for the bubbles to dissolve into the melt.

Additional experimental work is required to verify whether the one sample analyzed

for each oven temperature is representative of all molded parts produced under similar

conditions.
 54
CHAPTER FIVE

CONCLUSIONS

Rotational molding involves powder tumbling, melting, distribution of polymer melt

and cooling to form a solid part. The bench-scale molding machine built in our laboratory

was found to be a useful tool for studying the densification process and can provide

valuable information about molding cycle.

The density distribution across molded parts is an important characteristic for

rotational molding applications. The density is directly associated with the mechanical

properties of the molded part and is controlled in part by the densification process, and in

part by the solidification process. With the present densimeter, it is recommended that

larger volume part should be used for a more accurate result. Density measurements show

good repeatability. The oven temperature was found to have a significant effect on the

density profiles. The variations in the density with the axial position in the molded parts

were more pronounced for parts produced at high oven temperatures. When maintaining

constant temperature, small variations in the molding heating time seemed to have

important effects on the density profiles. The powder characteristics also were found to

have a pronounced effect on the density of the molded parts. Powders with very high fine

content produced parts with lower density and higher bubble content.

The presence of bubbles in the melt is intrinsic to the rotational molding process.

Variations in the bubble size and size distribution with respect to axial position along the

length of the mold were observed. Higher number and larger bubbles were seen at

positions close to the shaft and close to the window.

 The results presented in this thesis are mainly preliminary. These results are further

confirmed by theories about polymer sintering and polymer melt densification although

the uni-axial rotational molding machine has its limitations.

 56
REFERENCES

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 57
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21. R. W. Hopper, "Coalescence of Two Equal Cylinders: Exact Results for Creeping
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22. R. W. Hopper, "Plane Stokes Flow Driven by Capillarity on a Free Surface", J.

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24. N . Rosenzweig and M . Narkis, "Coalescence Phenomenology of Spherical Polymer

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25. N . Rosenzweig and M . Narkis, "Dimension Variations of Two Spherical Polymer

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PhD thesis, Eindhoven Univ. of Technology, The Netherlands (1994).
 58

28. C. T. Bellehumeur, "Polymer Sintering and Its Role in Rotational Molding", PhD
thesis, Chemical Engineering, McMaster University, Hamilton, Canada (1997).

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model assessment of polymer sintering", Polymer Engineering and Science, Mid-
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30. O. Pokluda, C. T. Bellehumeur and J. Vlachopoulos, "Modification of Frenkel's

model for sintering", AIChE Journal, December 1997, Vol. 43, No. 12, p3253-3256.

31. C. T. Bellehumeur, "Combined effect of polymer sintering and heat transfer in

rotational molding", A N T E C 9 9 , pi446-1450.

32. M . Weber and R. Gonzales, "Viscoelstic properties of rotational molding resins",

ANTEC'99,pl468-1470.

33. M . Kontopoulou, M . Bisaría and J. Vlachopoulos, " A n experimental study of

rotational molding of polypropylene/polyethylene copolymers", hit. Polymer.
Process, 12 (1997), pl65-173.

34. S. A . G. Castellanos, "Effect of molecular structure on the sintering of ethylene/a-

olefin copolymers", MSc. Thesis. University of Calgary, Canada. August, 2001.

35. P. Y . Kelly, " A microscopic examination of rotomolded polyethylene", Du Pont

Canada Inc.

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37. L. X u and R. J. Crawford, "Analysis of the formation and removal of gas bubbles in
rotationally molded thermoplastics", Journal of Materials Science, Vol. 28, 1993,
p2067-2074.

38. L . Xu, R. J. Crawford and A. G. spence, "Simulated bubble removal under normal
rotational molding conditions", Rotation/Fall, 1995, p9-12.

39. R. J. Crawford and A. G. spence, "Formation and removal of gas bubbles in

rotomolded products", Polymer Processing Society IX Annual Meeting, Manchester,
U K , April, 1993, 10-06.

40. A . G. Spence and R. J. Crawford, "Simulated bubble removal under pressurized

rotational molding conditions", Rotation/Fall, 1995, pl7-23.

41. G. Gogos, "Bubble removal in rotational molding", Preprints of the rotational

molding topical conference, June 6-8, 1999. Strongsville, Ohio. pl21-133.
 59

42. M . Kontopoulou and J. Vlachopoulos, "Bubble dissolution in molten polymers and

its role in rotational molding", Polymer Engineering and Science, Vol. 39, No. 7
(1999), p i 189-1198.

43. J. S. Tiang, "Development of a Numerical Simulation of Bubble Formation and

Dissolution in Rotational Molding", Internship Report, Department of Chemical &
Petroleum Engineering, University of Calgary, July, 2000.

44. J. McDaid and R. J. Crawford, "The grinding of polyethylene powders for use in
rotational molding", ANTEC'98, p i 152-1155.

45. R. J. Crawford, "Rotational molding of plastics", Prog. Robber Plast. Tech. Vol. 6,
(1) 1990,pl-29.

46. J. L. Throne, "Powder flow during rotational molding", ANTEC'2002.

47. R.J. Crawford, A. G. Spence and C. Silva, "effects of pigmentation on the impact
strength of rotationally molded polyethylene", A N T E C ' 9 6 , p3253-3258.

48. B. Muller, "Carbon black interaction with U V absorbers", Preprints of the rotational
molding topical conference, June 6-8, 1999. Strongsville, Ohio. p35-39.

49. P. Defranco, "Color in rotational molding: Directly moldable liquid colors",

Preprints of the rotational molding topical conference, June 6-8, 1999. Strongsville,
Ohio. p41-56.

50. B . Wiseley, "Fibres in polyethylene rotomolded parts", Preprints of the rotational

molding topical conference, June 6-8, 1999. Strongsville, Ohio. p27-32.

51. B. I. Chaudhary, E. Takacs and J. Vlachopoulos, "Processing enhancers for

rotational molding of polyethylene", Polymer Engineering and Science, October
2001, vol. 41, No. 10, pl731-1742.

52. A , Spence, "Investigation of the rheological properties of rotomolding resins",

ANTEC'99,pl482-1486.

53. M . J. Murphy, D. J. Martin, R. Truss, and P. Halley, "Improving polyethylene

performance - The use of nanocomposites in Ziegler-Natta polyethylene for
rotational molding", ANTEC'2002.

54. D. W. Sun and R. J. Crawford, "Analysis of the effects of internal heating and
cooling during the rotational molding of plastics", Polymer Engineering and Science,
Mid-February 1993, vol. 33, No. 3, pl32-139.
 60
55. S. O'Neill and R. J. Crawdord, "Investigation of cooling during rotational molding",
A R M Conference Report - Vienna 1996.

56. A . Spence, "Roto-blow molding, a rotational molding hybrid", ANTEC'98, PI 121-

1125.

57. C. H . Chen, J. L . White and Y . Ohta, "Mold pressurization as a method to reduce

warpage in rotational molding of polyethylene", Polymer Engineering and Science,
Mid-December 1990, Vol. 30, No. 23, pl523-1528.

58. K . Evans, "Using vacuum in rotational molding improves impact properties at low
temperatures and reduces cycle time", Preprints of the rotational molding topical
conference, June 6-8, 1999. Strongsville, Ohio. pl-6.

59. E. Harkin-Jones and R. J. Crawford, "rotational molding of liquid plastic system: A n

assessment of material moldability", Advances in Polymer Technology, Vol. No. 1,
1996,p71-100.

60. E. Harkin-Jones and R. J. Crawford, "Guidelines for the rotational molding of liquid
polymers", A N T E C ' 9 8 , p i 148-1151.

61. N . Corrigan, E. Harkin-Jones and R. J. Crawford, "Rotational molding of a

dicyclopentadiene reactive liquid polymer", ANTEC'2002.

62. G. Liu, C. B. Park and J. A . Lefas, "production of low-density L L D P E foams in

rotational molding", Polymer Engineering and Science, December 1998, Vol. 38,
No. 12,pl997-2009.

63. R. Pop-Iliev, G. Liu and J. A . Lefas, "Rotational foam molding of polyethylene and
polypropylene", Preprints of the rotational molding topical conference, June 6-8,
1999. Strongsville, Ohio. p95-104.

64. E. Takacs, J. Vlachopoulos and C. Rosenbusch, "Foaming with microspheres in

rotational molding", ANTEC'2002.

65. B. G. Wisley and R. J. Crawford, "Physical properties of laminates made from

L L D P E and cross-linkable HDPE by the rotational molding process",
Rotati on/summer 1996, p i 7-25.

66. R. J. Crawford and P. J. Nugent, " A new process control system for rotational
molding", Plastics, Rubber and Composites Processing and Applications, Vol.17,
N o . l , 1992, p23-31.

67. R. Pop-Iliev and C. B. Park, "Single-step rotational molding of skin-surrounded

polyethylene foams", ANTEC'2002.
 61

68. S. H . Teoh, K. K . Sin, L. S. Chan and C. C. Hang, "Computer controlled liquid

rotational molding of medical prostheses", Rotation/Fall, 1994, 10-16.

69. S. H . Teoh and C. Y . Lau, "Computer controlled rotational molding of a hollow

femur for 3-D photo-elastic analysis", Intern. Polymer Processing XIV No.4, 1999,
p370-376.

70. J. Fawcett, "3D molding and design", Preprints of the rotational molding topical
conference, June 6-8, 1999. Strongsville, Ohio, p i 15-120.

71. R. J. Crawford and P. J. Nugent, "Impact strength of rotational molded polyethylene

articles", Plastics, Rubber and Composites Processing and Applications, No. 17,
1992,p33-41.

72. C. T. Bellehumeur and J. Tiang, "Simulation of non-isothermal melt densification of

polyethylene in rotational molding", Polym. Eng. Sci., vol. 42, 2002, p215.
 62
APPENDICES

EXPERIMENTAL PROCEDURES

A- UNI-AXIAL BENCH-SCALE MOLDING MACHINE

Preheating of Oven

1-1 Make sure the oven is closed with an extra insulation.

1-2 Connect the power line with the oven.
1-3 Turn the main power on.
1-4 Turn the two fans on by turning the fan controls to position ' 1 ' , which
corresponding to a speed of approximately 1600 rpm.
1-5 Controller parameters set up. In order to get a good repeatability, normally do not
change the controller set up. If you want to change the parameters, Please consult
the Series 93 User's Manual. The pbl (proportional band) value is preferred to set
small value (currently pbl =3) for quick reaction of oven temperature changes.
1-6 Set the oven temperature to an appropriate one (See Tablel) for corresponding
oven temperature. This is to compensate for the heat loss when the mold is being
placed into the oven.

• Thermocouple 1 controls the oven temperature.

• Thermocouple 3 measures the air temperature inside the mold.

• Thermocouple 4 is connected to the safety to make sure the oven is not overheated.
Always keep thermocouple 4 in the oven.
For the detail locations of the thermocouples, see Figure 3
Table 2. Oven temperature and corresponding preset temperature
Required Oven Temperature (°C) 250 350 425
Preset Temperature (°C) 330 480 590
1-7 During the oven preheating, prepare the mold for rotational molding.
 63
Mold Preparation
2-1 Make sure the mold is completely clean, without any traces of prior mold resin.
2-2 Weight required amount of resin and carefully fill the mold with resin. Tight the
cover to close the mold.
2-3 Roll the mold on a flat surface to equally distribute the resin along the axial
position.
2-4 Attach the mold to shaft and secure it in place by tightening the screws located
where the shaft inserts into the mold.
2- 5 Start rotating the shaft at a required speed.

Data Acquisition
3- 1 Create a new Excel worksheet file with suitable name for the new experiment data.
3-2 Start Fplogger program.
3-3 The program will ask for a file name to save the data. Use a dummy name "
test_dec5" as the file name.
3-4 Change the temperature axis to a suitable scale (normally, 500°C)
3- 5 Change the Advice rate (time interval for recording data) to 10000 ms and stop the
recording.

Starting Experiment
4- 1 Make sure that the oven reaches the required temperature. Also make sure that the
thermocouple 3 is inserted inside the mold.
4-2 Click on icon '=>' on Fplogger program, save the new file under the file name
created in step 3-1.

4-3 Quickly remove the insulation lid and roll the oven over the mold, cover the oven
properly. If the cover rotates, block it with a pin.
**Note: A , This operation should be done quickly to reduce the heat loss.
B, Don't roll the oven past the mark (avoid hitting mold on the fans) damaging the
fans.
4-4 Reduce the set temperature to the required oven temperature.
 64
4-5 To control the peak air temperature inside the mold within 196-200°C, the mold
needs to be taken out of the oven at different temperatures showed on
thermocouple 3 for different oven temperature. Reference temperatures at which
the mold is moved out of the oven are given in the following table.
Oven temperature (°C) 250 350 425
Moved out temperature (°C) 197-198 172-174 132-134

4-6 When the mold is taken out, turn on the pedestal fan ('3' speed) and position it so
that it's facing the mold.
4-7 Once the inside air temperature has cooled down to about 50°C, turn off the
pedestal fan and stop the rotation.
4- 8 Remove the mold.

B- PROCEDURE FOR RS LAB 40

5- 1. Switch on the main power supply on the wall (the right one)
5-2. Turn on the machine power located at the right top corner of the first door at the
back of the oven. As soon as this switch is turned on the safety breakers for the
power supply to the rotating axes goes off. The two green buttons behind the
second door underneath the label 'Major Axis" and 'Minor Axis' has to be
pressed in two times to ensure power supply to the axes.
5-3. Start the computer and login.
5-4. Prepare the powder for the rotomolding process.
5-5. Start the RS L A B 40 program, and go to D A T A E N T R Y section from the M A I N
MENU.
5-6. Set up the desired parameters for the cycle. Note: Don't put zero time for the steps
that you don't want to run (at least put a value of one second).
5-7. Go back to M A I N M E N U and then to M O L D B A L A N C I N G section.

•=> Adjust the mold to the suitable position and put the powder in
•=> Insert the thermal couple to the suitable position
•=> Close the mold tightly
 65

5-8. Carefully insert all the thermocouples to the corresponding numbers in the Data
Logger. Adjust the position of the mold to fit the Temperature Recorder in.
5-9. Again start the mold motion and check for the proper fitting of the data logger.
5-10. Check if the oven temperature has been reached.

5-11. If the oven is at its set point, switch on the data logger and remove the switch.

5-12. Start the Rotomolding Cycle by pressing the start button at the O V E N menu.

5-13. Monitor the mold-balancing trend from the graph (must be a straight line for a
balanced mold). If there is any problem it has to be fixed.

5-14. Monitor the entire Process.

5-15. After the cooling process is over, carefully remove the data logger.

5-16. Attach the CorrecTemp Data Logger to the computer and save the file in the Hard
Disc as soon as possible.

5-17. Download the molding part.

5- 18. If all the experiments are finished, log off the computer and turn of the power
supply.

Setting up the Data Logger on STP LAB40

6- 1. Creating a file to store data:
6-2. Plug in the Power Cord for the data Logger in the A C Adapter Port and attach the
cord connecting the Computer in the serial Interface port.
6-3. Connect the port to start switch port (the port right to 8 thermocouple port)
6-4. Torn on the ON/OFF switch.
6-5. Startup the Stphost program.
6-6. There are two icons: One is 'open PDT to clone', with which you can produce a
new PDT file to run. When you finish clone, give the new PDT file a new name.
6-7. The other is 'open PDT to run', with which you can select an old PDT file to R U N .
6-8. After you click 'ok' the data logger will erase the previous memory and then create
a file to record the data.
6-9. Don't forget to set up the run time and the logging rate for the experiment.
 66
6-10 The red light in the start switch will glow up i f every thing has been done
properly.
6-11 Remove the power cord and the serial Interface port.
6- 13 The data Logger is now ready for the experiment. Don't turn off the switch until
the experiment is ready to begin. And remove the Start Switch before entering in
the oven cycle.

Retrieving the Data:

7- 1. Connect the power cord to the A C Adapter Port and serial Interface Port.
7-2. Click on the 'Retrieve data' icon to transfer the Data to the hard disc. Give the file
a new name and save it.
7-3. Turn off the ON/OFF switch to conserve battery life.

C- CUTTING ROTOMOLDED SAMPLES FOR TESTING THICKNESS

1-1 Remove the molded part from the mold. On the molded part, indicate where the
window of the mold was located. This location is important for future use.
1-2 Using a sharp utility knife cut the molded part along its height to obtain 4-6 equal
parts (see Figure 5).
1-3 Once 4-6 parts are obtained, remove the flash with a knife.
1-4 Label each of the 4-6 parts with a number, such as ,1,2,3,4,5,6.
1- 5 Strip a whole length sample for each part for bubble count.

D- TESTING ROTOMOLDED SAMPLES FOR THICKNESS

2- 1 Position a ruler along the length of the sample starting from the shaft end. The
shaft end is opposite to the window (window location was labeled in step 1).
2-2 Using the caliper measure the thickness starting from the shaft. Record the
thickness every 0.5cm until the end of the sample is reached.
2-3 Repeat the measurement with the three remaining samples.
 67

E- CUTTING ROTOMOLDED SAMPLES FOR DENSITY MEASUREMENTS

3-1. Cut the each part produced from step 1-3 into 3 or 6 equal parts along the length.
3- 2. Label each part with a number and letter such as 1 A , IB and 1C, or 1 A , IB, 1C,
ID, IE and IF, respectively (see Figure 5).

F- DENSITY MEASUREMENTS

4- 1. Pour distilled water up to the line on water tank, then put it on holder gently.
4-2. Put sensor on support.
4-3. Make sure that the bottom of sensor is correctly positioned on the support, and
basket sinks in water. If there are air bubbles adhering to the basket in water, shake
the basket with TWEEZERS to remove them. Put the steel angle in the water.
4-4. Turn on the powder and allow MD-200s to warm up for 10 minutes
4-5. Follow the Calibration procedures outlined on page 4 of the Electronic Densimeter
MD-200s Instruction Manual.
4-6. Follow the "Solid Mode Operation" Procedure on page 6 of the Electronic
Densimeter MD-200s Instruction Manual, to determine the density of each molded
part.
4-7. Once one set of density measurements is obtained, dry the samples with a
Kimwipe.
4-8. Repeat the density measurements if necessary, making sure that the samples are
dry from the previous test.
4- 9. The repeatabilities of the density measurement are given in Table 5 and Table 6

G- DETERMINING BUBBLES IN T H E ROTOMOLDED PART

5- 1. Mount the plastic strip on a glass slide and hold it in place with some scotch tape.
Make sure the mold surface matches the up boundary of the image.
 68
5-2. Switch on the microscope. Make sure the transmitted light and the 1.25X lens are
used.
5-3. Carefully place the glass slide on the stage. Adjust the slide so that the sample can
be observed from the observation window. Position the plastic strip so images will
first be taken from the shaft side.
5-4. Load the Image-Pro Plus software. Select Acquire - Setup Acquire to open the
Pro Series Capture 128 window. Under the sub-menu Setup, select Configure -
Pro Series Monochrome as the current integrating camera. Make sure the 8-Bit
gray scale Acq. box is checked
5-5. Under the sub-menu Image, select Start Preview. Adjust the focus and light
intensity to get a clear view of the bubble layer on the computer screen. The
background should be white and the bubbles should be as dark as possible, to
obtain a good analysis of the picture. Adjust the edge of the molded part next to
the mold surface lining up with top of the computer screen display.
5-6. Once a good image is obtained on the computer screen, press Stop Preview.
Close the image, and press Yes when asked to save changes. Save the file in a
directory and name it appropriately.
5-7. Move the sample to a new position next to the old one and repeat 5-5
5-8. Repeat step 5-5, to obtain pictures of the whole sample.
5-9. Set the spatial calibration to 1.25 X reduced 2 to carry out the image analysis
5-10. Open the picture that you want to analyze.
5-11. Use the square AOI to select the interesting area, click on the icon of count/size.
5-12. Under the sub-menu Count/Size, from File menu, select load settings. Load the
file 'testbubble'. This step is not mandating. You can define specific measurement
depending on requirement and save it as a new file and load it when needed.
5-13. Press Count. From the select ranges, adjust the color range to make all the
bubbles in the AOI out of the background.
5-14. Select proper AOI for rest bubbles which are not included in the square AOI.
When finish with one bubble, select add and new AOI for the rest. Repeat the
process until all bubbles are included.
 69
5-15. Under the sub-menu Count/Size, from Edit menu, select covert AOI to objects.
5-16. Export the count result to Excel by selecting DDE to Excel from the file menu.
5- 17. From the free measurement menu, select the square tool to measure the whole
image area and press on export now. A l l data are exported to Excel.

H- PARTICLE SIZE DISTRIBUTION (SIEVE ANALYSIS)(ASTM D 1921-96)

6- 1. Make sure the sieves and the pan are clean. If not, clean it with brush and vacuum
cleaner.
6-2. Weight the sieves and the pan, and record the data.
6-3. Put the sieves in a size decreasing order and the pan at the bottom.
6-4. Weight 50g of sample to the nearest 0.1 g and transfer it to the top of the stack.
6-5. Cover the stack and place it in the mechanical sieve shaker. Start the shaker and
run for 10 minutes.
6-6. After shaking, carefully separate the stack of sieves beginning at the top and
weight each sieve with powder to the nearest O.lg. Determine the weight of the
powder in each sieve and pan.
6-7. Calculate particle size distribution.
6-8. Calculate the mean particle size as

where :
D m = mean particle diameter, jum,
P¡ = material retained on each sieve, %, and
Dj = average particle size of material on sieve, fjm.

I- OVEN TEMPERATURE CONTROL AND OVEN TEMPERATURE

DISTRIBUTION
Oven temperature responses to different proportional band values are shown in Figure 21.
Temperature spatial distribution inside the oven is illustrated in Figure 22
 Table 5 Repeatability of density measurement

Sample No. 020221DB

Molding conditions: Resin: TR0242, 50% 35-40mesh +50% 70-100mesh,

shot weight: 100g, oven temperature: 425°C, rotating speed: 5rpm

Test date 24-Feb-02

Relative distance to shaft side

0.1 0.2 0.4 0.6 0.7 0.9

1 0.918 0.922 0.929 0.933 0.933 0.925

O 53
sample numb'
Radical directi

2 0.918 0.921 0.928 0.932 0.933 0.924

3 0.916 0.919 0.927 0.933 0.932 0.923

4 0.917 0.92 0.929 0.932 0.932 0.922

Average 0.917 0.921 0.928 0.933 0.933 0.924

SDEV 0.0019 0.0026 0.0019 0.0012 0.0012 0.0026

(95% confidence)
Test date 28-Feb-02

Relative distance to shaft side

0.1 0.2 0.4 0.6 0.7 0.9

1 0.915 0.921 0.931 0.933 0.932 0.924

O cu
dical idirecti
mple numb

2 0.915 0.923 0.928 0.931 0.934 0.924

3 0.917 0.921 0.93 0.931 0.931 0.925

c3 co 4 0.915 0.919 0.929 0.934 0.93 0.923

Average 0.916 0.921 0.930 0.932 0.932 0.924

SDEV 0.0020 0.0033 0.0026 0.0030 0.0034 0.0016

(95% confidence)
 Table 6 Repeatability of density measurement

Sample No. 02022IBB

Molding conditions: Resin: TR0242, 40-50mesh, shot weight: 100g, oven temperature:

350°C, rotating speed: 5rpm.

Test date 24-Feb-02

Relative distance to shaft side

0.1 0.2 0.4 0.6 0.7 0.9

1 0.918 0.92 0.921 0.924 0.923 0.92

Radical direction
sample number

2 0.918 0.918 0.921 0.924 0.924 0.917

3 0.918 0.919 0.923 0.925 0.924 0.919

4 0.917 0.918 0.921 0.923 0.923 0.919

Average 0.918 0.919 0.922 0.924 0.924 0.919

SDEV 0.0010 0.0019 0.0020 0.0016 0.0012 0.0025

(95% confidence)
Test date 28-Feb-02

Relative distance to shaft side

0.1 0.2 0.4 0.6 0.7 0.9

1 0.918 0.916 0.921 0.924 0.924 0.919

Radical direction
sample number

2 0.918 0.919 0.92 0.925 0.922 0.919

3 0.92 0.92 0.921 0.925 0.924 0.917

4 0.917 0.92 0.922 0.925 0.922 0.919

Average 0.918 0.919 0.921 0.925 0.923 0.919

SDEV 0.0025 0.0038 0.0016 0.0010 0.0023 0.0020

(95% confidence)
 o 325
I-

300 -I 1 1 1 , 1

0 1 2 3 4 5 6
Time (min)

Figure 21 The temperature r e s p o n s e s for different pbl values

S3
 73

Figure 22(a) Temperature Profiles at Different Positions

300

0 -\ , i , !

0 5 10 15 20

Time (min)

F i g u r e 22(b) T h e A v e r a g e T e m p e r a t u r e of the O v e n
(with m o l d in)