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Assessment of processing techniques for
Orthopaedic Composites
Ghazal Hedjazi

Ghazal Hedjazi
Master thesis
Subject Category: Biotechology
Series Number Biotechnology 6/2009
University College of Borås
School of Engineering
SE-501 90 BORÅS
Telephone +46 033 435 4640
Examiner: Mikael Skrivars
Supervisor: Karri Airola
Client: The University College of Borås; European Research Project NEWBONE
Date: 15.09.2009
Keyword: Orthopedic composites, processing techniques, Result comparison

Summary
orthopaedic a of lot have been implants Titanium, Metallic in widely applications. used Ceramics,
bones alloys grade designed inserted artificial medical as titanium other large and in are metal
healing bars attached of joints. in fractured and Plates facilitate also order bones to to are
of The the so implants of and however disadvantages corrosion release bones. are metal ions,
closer a is density which have orthopaedic new need for there composites, finding materials like
too. natural the to bone
and and on project it part of This project is manufacturing is based the NEWBONE European
properties. reinforced of glass processing of fiber and the composite assessment its
The is parts to composite the dimensions manufacture in designs lab of the project goal in and different
which are chemical for tests. suitable and mechanical
The medical work processing with composites, the medical methods theoretical the and devices, deals
reinforcement fibers PEEK and carbon composites, and plastics, other materials. medical of
glass resin. content, curing The fibers dental with void The are glass impregnated residual fiber
and properties chemical by are standard and estimated ASTM content methods. mechanical
resented according composite mechanically and to Results performance chemically of evaluation are
best and of future choice show use orthopaedic to composite parts of order improve in the
applications.

2 - -
of Table Contents
i ………………………………………………………………………………………... Summary
Contents of ..........................................................................................................................3 Table
Abbreviations..................................................................................................................6 of Index
part.................................................................................................................7 I: Theoretical Part
.................................................................................................................7 1. Introduction/preface
1.1 ...........................................................................................................................7 Background
1.1.1 Medical composites: ...............................................................................................................7
1.1.2 ..................................................................................................................................7 History
1.1.3 Market...................................................................................................................................7
Problem 1.2 discussion............................................................................................................9
Biocompatible ........................................................................................................9 ceramics 1.2.1
Polymers............................................................................................................................11 1.2.2
Composites .........................................................................................................................11 1.2.3
in Composites 2. orthopedic........................................................................................12 material
on matrix.................................................................................13 based composites Bioactive 2.1
.........................................................................................13 Polymeric biomaterial Composite 2.1.1
orthopedic:..............................................................13 2.2 materials Application composite in of
...................................................................14 plates composite Polymeric materials as bone 2.2.1 [1]
2.2.2 composites as intramedullary nails: Polymeric ......................................................................15
The bone of in replacements: 2.3 advanced composites ..................................................16 types
Advantages polymeric 2.4 ...................................................................17 composite of materials:
Structural 3. composites ......................................................................18 in reinforced Material
Materials matrix phase: 3.1 as ..................................................................................18 Polymeric
Thermoplastic 3.1.1 polymers:.......................................................................................................18
polymers: ......................................................................................................18 3.1.2 Thermosetting
Resorbable 3.1.3 materials.............................................................................................................18
composites 3.1.4 ...................................................................................................18 carbon Carbon/
composites. matrix ..................................................................................................18 Ceramic 3.1.5
phase:........................................................................................18 3.2 as Material Reinforcement
..................................................................19 orthopedic material Reinforcing 3.3 composites: in
........................................................................................................................19 Carbon 3.3.1 fibers
- - 4
3.3.2 Glass fibers..........................................................................................................................19
3.3.3 Bioglass:..............................................................................................................................20
Aramid as: such 3.3.4 fibers Kevlar®............................................................................................20
process Fabrication of 4. composites......................................................................20 orthopedic
of material........................................................................................20 4.1 the and Design device
of aspects 4.1.1 composites:.......................................................................20 implantable Biological
of 4.1.2 composite: ......................................................................21 implantable Mechanical aspects
Processing methods..............................................................................................................21 4.2
up: 4.2.1 .........................................................................................................................21 Hand lay
........................................................................................................23 moulding: 4.2.2 Compression
technique:..................................................................................................24 4.2.3 Vacuum bagging
......................................................................................................25 moulding 4.2.4 Injection Resin
4.2.5 injection Vacuum .................................................................................................26 moulding:
4.3 Sandwich ........................................................................................28 structure composite: of
4.4 ................................................................................................................................29 Curing:
4.4.1 ...........................................................................................29 Curing of thermoset composites:
Part ........................................................................................................30 II: Experimental part:
5. Method: and Material .............................................................................................................30
5.1 ...................................................................................................................30 Reinforcements:
Resin matrix ............................................................................................................32 5.2 or part:
Constituents curing ........................................................................................32 of 5.2.1 resin dental
Procedure resin for batch preparation: ...................................................................................33 5.2.2
Open moulding 5.3 resin: of ......................................................................................................34
and Manufacturing the of .....................................................................35 6. samples: Grouping
Group 6.1 technique Processing ............................................................................................36 1:
2: Group Wovens vs. structure:....................................37 6.2 vs. fibres Unidirectional sandwich
Comparison 6.3 ...........................................40 different 3: samples: woven: Sandwich Group of
4: 6.4 60ºC........................................41 Room Processing vs. Temperature: Temperature Group
Effect thickness:....................................................................................42 Group5: of sample 6.5
Effect size:.............................................................................................43 Group6: of mould 6.6.
Characterization: ....................................................................................................................44 7.
Visual ..............................................................................................................44 observation: 7.1
Resin time:...................................................................................................................44 Flow 7.1.1
Air appearance: bubble .........................................................................................................46 7.1.2
5 - -
Chemical tests: ....................................................................................................................48 7.2.
Gravimetric Thermo 7.2.1 (TGA)..................................................................................48 Analysis
Mechanical Tests 7.3. ................................................................................................................50
Ignition content/ Fiber ............................................................................50 measurement: 7.3.1. loss
Void 7.3.2. .......................................................................................................................52 content:
Density 7.3.3. ...............................................................................................................................53
Results 8. .....................................................................................................................................57
..................................................................................................................................59 References:

Index Abbreviations of
carbone CF fiber
C carbone
:kelvar KF fibers
PMMA polymethylmethacrylate
PS polysulfone
polypropylene PP
weight ultra-high-molecular polyethylene UHMWPE
poly(L-DL-lactide) PLDLA
poly(L-lactic PLLA acid)
polgelycolic acid PGA
polycarbonate PC
polyetheretherketone PEEK
hydroxyapetite HA
polymethacrylate PMA
glycidyl Bis-GMA A methacrylate bis-phenol
Polyurethane PU
polytetrafluoroethylene PTFE
polyethyleneterephthalate PET
poltethylacrylate PEA
rubber SR silicon
glycol PELA of polyethylene block co-polymer acid lactic and
GF fibers glass
LCP crystalline liquid polymer
PHB polyhydroxybutyrate
PEG Polethyleneglycol
PE ethylene Poly
PA Polyacetal
PLA acid) poly(lactic
MPa Megapascal
porosity of reinforcement
permeability reinforcement K of
of resin viscosity
flow distance L
applied pressure p
magnetic MRI imaging resonance
of Swedish of THS Textiles School Borås University The College

I: Part Theoretical part
Introduction/preface 1.
Background 1.1
Medical composites: 1.1.1
Matrix two phases: Reinforcement. reinforcement and materials of The Composite are made
more phase and strength matrix and fills stiffness. it gives the
can application this inside and In inserted orthopaedic 2phase the can bone mimic the be natural
applications and composites medicine to a lot it bone support Medical from in of have inside[4].
whereas their this orthopaedic. experimental the work orthopaedic In we thesis consider application
orthopaedic manufacturing of of work composite the application assesses for methods medical part
of bone Biomedical / as materials group orthopaedic composites belong to implants. a
functions). their tissues substitute natural the and can (Biomaterial perform body biomaterials in called
[1]
1.1.2 History
Based it that found had thesis, done the biomaterials ancient on was since used research for been this
civilization time.
implantable biomaterial to time used such as: be at Some that found was
- implants, valves. heart Joint 1 plates, replacement, dental bone
- hearts- Artificial tubes. blood 2
- eyes-noses Egyptian. 3 Artificial by [1]
at that tissue Some of implantable age like: some natural material made biomaterials were wood,
living of zinc, organs, iron. gold,
1.1.3 Market
from the According 1995 is billion it in to of 12 London’s biomaterial, a institute market report of
this increasing and biomaterial dollar the in is year for range annually[1]. market per 7-12% of
8 - -
composites that Regarding their and in biomaterial body fact perform the medical the in function
be contact structures close properties to tissues, their should with tissues much as as and living as
possible.
that stress the almost amount of suffer is orthopaedic For 4 composites MPa, in bones example,
during this up to 40-80 for can MPa. tendons, more but other daily work, tissues like be
3000N of average jumping on increase the amount almost joint is during hip The and load can up
and to is kind can of And stress be 10000N. in amount this not changed different constant clearly
[1] activities. of
have implants many different for made of been bone of materials composite various kind Therefore,
material and manufacturing during could But of materials that last decades. processing mimic
case and of functions bone the still structures interest. the is
are Composites high stiffness, with and strength flexural reviewed strength high and biocompatibility
biomechanical ideal an group of behaviour. occasionally have as materials potential to a
between find 30 done interaction to and Since last researches years many the implanted been action had
inserted it obvious that living organs. to and biomaterial be made materials This those
compatible body found of Some be be should implanted composites were inside to the and compatible.
inside and in of the and surrounded them contact with the some some tissues body had
failures, too. bodies were in different reaction observed different conditions and but
In like considered biocompatibility should be manufacturing of composite some factors orthopaedic
of composite.
Biocompatibility:
the in the tissue. composite and host material to ability interact with Is perform living of contact
reach they should To structurally goal physically composites, orthopaedic (surface) and this be for
compatible:
• Surface compatibility:
of material and surface The ,physical optimum chemical have an biocompatible biological should
with tissue [1] compatibility host . organ. or
• Structural compatibility:
- 9 -
biomaterial optimum also should matching mechanical performance with a The in exhibit contact
living tissue.
the minimum well strength that this the includes load means the And of implant transmission; as as
interface mismatch.
compatibility compatibility be of ideal and an both surface structural For should implant-tissue,
manufacturing must considered. and in this and of composite medical characterization be fact achieved
have represent best best made and are of materials 2 to the mechanical function Composites constituent
strength-fatigue and as and the resistance properties also best such biocompatibility stiffness
even than is more mechanical important which properties.

Theoretical I: part Part
Introduction/preface 1.
Background 1.1
composites: 1.1.1 Medical
reinforcement are The Composite of made materials Reinforcement. two Matrix phases: and
stiffness. the phase matrix more strength and fills and gives it
the inserted natural this orthopaedic the can can application be In mimic and bone inside 2phase
bone a inside[4]. Medical medicine applications composites in support it and have to of from lot
In thesis orthopaedic. orthopaedic whereas this work consider their application experimental the we
work of manufacturing orthopaedic the composite methods part medical of assesses for application
/ implants. as materials bone of orthopaedic belong a composites Biomedical to group
substitute called tissues biomaterials the and (Biomaterial perform their can in functions). natural body
[1]
1.1.2 History
thesis, found this research had was that done since Based been biomaterials for it on used the ancient
civilization time.
used that implantable be at such time was Some found to as: biomaterial
dental replacement, heart implants, Joint 1 bone valves. - plates,
blood 2 - tubes. hearts- Artificial
Egyptian. 3 eyes-noses [1] - Artificial by
like: wood, material tissue made Some some that at were age of implantable natural biomaterials
gold, organs, zinc, of living iron.
Market 1.1.3
billion it report London’s institute of of market is to in the 1995 According a 12 biomaterial, from
dollar is increasing market 7-12% year range per of the in and for this biomaterial annually[1].
- 8 -
the in their in Regarding that medical the and function body fact composites biomaterial perform
tissues, tissues as to structures living with much contact should and close properties their be as as
possible.
orthopaedic of bones 4 in For is amount composites almost example, MPa, suffer that stress the
tissues tendons, MPa. 40-80 during daily be can for this more work, up to like other but
of on up jumping almost and is joint amount the hip can 3000N during increase load average The
clearly amount kind different constant can not is And of stress be and in changed this 10000N. to
of activities. [1]
kind many composite Therefore, different bone have of materials of various for been implants made
decades. mimic of during manufacturing materials and could But material last that processing
and interest. still bone is the structures of functions case the
and strength reviewed with flexural biocompatibility high strength stiffness, high and Composites are
group ideal behaviour. as an to a potential of materials have occasionally biomechanical
researches and implanted 30 action to last many been done the had between find interaction years Since
This that organs. living made it biomaterial those materials and obvious inserted be to
should composites body the inside compatible. and of were implanted be compatible to be found Some
with the some in and some them surrounded and of body contact the had inside tissues
in different conditions reaction were too. observed bodies but and failures, different
composite some be orthopaedic considered biocompatibility like factors manufacturing should In of
of composite.
Biocompatibility:
material the Is interact the contact with host and composite living ability to of in tissue. perform
composites, reach orthopaedic should they goal structurally To and this for (surface) physically be
compatible:
Surface • compatibility:
have biological optimum should ,physical and of surface an material biocompatible The chemical
tissue [1] organ. host . or compatibility with
Structural compatibility: •
9 - -
a in The mechanical should matching biomaterial exhibit contact also optimum with performance
tissue. living
as that And as the well strength implant means of this minimum load the includes transmission; the
mismatch. interface
both and of surface structural an For should compatibility be compatibility implant-tissue, ideal
medical characterization fact must achieved be considered. this of and composite and in manufacturing
constituent function represent and Composites best mechanical the 2 best of are made to materials have
stiffness resistance the also properties best biocompatibility and and as strength-fatigue such
important is which properties. more than mechanical even
Problem 1.2 discussion
bone many, For them been used of years with material different each some as implants, many had
and advantages shortcomings.
biomaterial Various implantable orthopaedic: in types of
as The used are: in materials now have orthopaedic biomaterials been that until
material -ceramic
-metals
biomaterial -polymeric
combination material. of previous material made can be of which -composite
ceramics Biocompatible 1.2.1
glass-carbone bioactive This group and Alumina-titania-zironica-bioglass includes hydroxyl or
glasses and appetite as and as well glass-ceramics. ceramic
to bioceramics. ago was It used 30 of since because be years biocompatible It is found called and
containing environment[2]. human chemical the similarity with (Ca+2- body like: ions They are
in like total Na+). Alumina, used replacement. Mg2+, K+, zirconia Some hip are ceramics
- - 10
and of their 2-1: implantable biomaterial properties Table Groups
Failures Material Properties
Ceramic
Alumina-titania-zironica-bioglass
hydroxyl or glass-carbone bioactive and
and appetite. Ceramic
-glass-ceramics glasses and
-biocompatible
corrosion -low
against -resistant
compressing
brittle -
fractures against -low strength
density -high
fabrication in - Difficulties
alloys: and Metal
-Gold
-Tantalum
and steel -Stainless
alloys. -Ti
alloys -Co-Cr (cobalt-chromium)
strength -high
stable -very
gnawing against
biocompatible - less
contact - Too tissue hard at
corrode - easy to
- high and density weight
- Ions allergy host in tissue. cause may emission
Table 2-2 and 10-20 materials higher are times that metallic Table show in 2-3 ceramic and
modulus using in failures than can lead natural to itself these bones. some case This materials.
One stiffness the that of arisen from the this has fact problems between been in orthopedic metal
ceramic to not bearing bone were tissue with the implants or less and load host in led match this
bone or to protection is implant called that stress compared “stress [1]. shielding`”
Table and Properties biomaterials[1] of 2-2: metallic ceramic
Material strength Tensile (Mpa) Modulus(Gpa)
Stainless 190 586 steel
Ti-alloy 965 116
Amalgam 58 30
Co-Cr 210 1085 alloy
Ceramic material
Alumina 380 300
Bioglass 35 42
Zirconia 220 820
Hydroxyapetite 92 50
- 11 -
2-3: Table of Mechanical bones[1] some properties
Tissue Modulus(Gpa) strength Tensile (Mpa)
Cortical bone(longitudinal 17.7 direction) 133
bone(transverse 52 12.8 Cortical direction)
Enamel 10 84.3
Cancellous 7.4 0.4 bone
Dentine 39.3 11.0
1.2.2 Polymers
properties, tissues mechanical this blood Regarding used in and to is material the soft vessels like
skin.
1.2.3 Composites
composite came 1980 in of Considering bone the The observed problems [3]. since using implant idea
the using materials previous failures higher materials, strength and with and composite from
similarity to develop. natural had more stiffness to and bone started
least one bioactive of constituent at medical (metal-polymer In material composites should be the
of composites or based their name ceramic). polymer)[ or on is matrix phase (metal-ceramic The
2].
bioactivity of composites, factor in In considered medical manufacturing is should a that be main
the choosing material.
Why composites:
strong Bones and clearly are have modules. hard as high Bones stiff a Human and tissue elastic
made crystals hydroxyapetite collagen and and fibers material naturally composite of are of structurally nano
sediment fibers[1]. collagen are in which
elastic high modulus hydroxyapetite is fibers and modulus collagen have low The elastic with
weight supports 70% stiffness almost bone. and of of and the the dry bone contain and
12 - -
material composite represent great fact, could this biocompatibility. Regarding
affected by which the the stress the can in applied the can body on bone It be is bone. of Density
stress is equal denser higher that said bone be to
be, normal Bone of bone. is less stress should it be If than weakening led can the stress to it the
with and break. impact, can tension-resistant not in condition the loading is high and
material 2. Composites orthopedic in
Orthopedic Figure 2-1: biomaterial
Orthopedic
Biomaterial
Ceramics
Alumina,Bioglass
Metals
steel,... stainless
Composites
Reinforcement Matrix
Polymer
matrix Metal
HA/Ti
matrix Ceramic
steel/HA stainless
fiber Carbon
Bioglass
fibers Glass
Thermoset Thermoplastics
- - 13

proved very choice bone composite good substitute Nowadays materials that are for and a it is
implant orthopedic surgeries. in
can be based Medical classified groups: bioactivity on in following composite
carbone/ PEEK - Bioinert: carbone/ carbone,
stainless HDPE, composites: steel/ bioglass, Ti-A6-4V - Bioactive HA/ HA/
TCP/ PLA, Bioresorbable - composites:TCP/ PHB[2].
on composites matrix 2.1 based Bioactive
following classified the the to groups: material they composite, in According used are in matrix
HA/Ti-6Al-4V matrix Metal composites:HA/Ti, •
Glass/HA(2) Ceramic • stainless matrix steel/HA, composites:
• Polymeric PEEK,HA/HDPE composites:
Using reinforced would choice material which is The be polymeric has a popular. best modulus lower
material high has polymeric modulus. which composite as material and low strength
2.1.1 Composite biomaterial Polymeric
to and found fewer better other failures composites have are groups are Polymeric to compared a
alternative substitutes which material as previous choice groups.
and are variable properties, - performances They composition. in and different
found They shapes and in can (films-fibers…) - different be forms
used material. liquid and some absorb also They be - fillers can as
composite materials in orthopedic: of 2.2 Application
applications variety As be was can before, they human applied body, the mentioned it they in of have
case consider or and we implantable In their in material. soft hard tissues in application our
in material bone as orthopedic implantable surgery.
fractures Bone
some The in possible are bone ways: repair fractures to different
- 14 -
fixation: External •
some need this is in tissue. no open to kept The In the fracture devices there procedure bone is
and as such material casts-splints.
The cotton made casting of of a composite and material consists calcium woven sulphate material
matrix glass such and as reinforcement and material fibers some polyesters.
• fixation: Internal
this using of fixation surgery implants and fracture bone is repaired. techniques In kind by the
on different bone fracture implants used be wires, as pins, screws, can Depending the some such
bone or plates intramedullary nails.
screws are fixation[1] common be and parts Steel-Ti made internal in most alloys and can of Plates
or Co-Cr alloys.
or Almost from surgery 2 removed years after are the screws body. and plates bone the the bone 1
can The plate. gets carry the less stress removing and after bone to easy break weak The and bone
less weakening from alloy by plates using Ti material is using with of less modulus (due Ti); to
modulus also to the bone is preferred. closer
material Their can and in polyester show be properties plate As PA-PTFE bone used. alternative
has not modulus low strength. that enough too and it
material stiffness and strength composite Therefore, polymeric high material with suitable as a the
is choice. best the
Polymeric as [1] materials composite plates bone 2.2.1
Non composite plates: –resorbable
in vivo strength condition stable change without in stiffness. This and and any material the is body in
made thermoset be materials. CF/ or thermoplastic Epoxy It epoxy- of can GF/ composite
In partially nonresorbable are some cured epoxy monomers (thermoset toxic material). material
reported.
CF/PMMA- Thermoplastic: (this material CF/PP-CF/PS-CF/PE-CF/Nylon_CF/PBT-CF/PEEK-
hydrolyze) and enough fatigue biocompatible is is to difficult and a rejection stiff resistant and it also
by carbon seen be of fibers has tissue not much. [1] to
gelicolic material body, degraded acid be or poly polylactic (PLA) acid- in can this (PGA) the
after period. certain a gets weaker
15 - -
resorbable plates: Fully bone
reinforcing poly-L composites lactic Example: of acid and They resorbable fibers are materials.
and glass fibers fibers. based calcium phosphate (PLLA)
Partially resorbable:
the are polymers some their material reinforced resorbable improve mechanical by properties To
and they fibers. partially as resorbable are Thus, resorbable) carbon called fibers- polymeric (non such
like CF/PLA composites. material,
composites as nails: intramedullary Polymeric 2.2.2
be bone long They used can bone fractures inside it. The nail inserted to are the and must fill in
body. the support be strong Intrarmedullary are weight nails of stainless steel of made to mostly
et composite, The GF/PEEK al. composite suggested Lin by was or for which that reason this is
better show properties more mechanical bone. and also biocompatibility in materials contact with
carbon this liquid discovery, fiber continued using of reinforced the After polymers crystalline was
intramedullary and strength et higher as al nails. be flexural to by have Kettune They used
to [1] bone. closer the modulus elastic
composite [1] orthopedic 2-1: in of Table polymeric Application material
Composite material Application
CF/LCP,CF/PEEK, GF/PEEK Intramedullary nails
ligaments PET/PHEMA.KF/PMA,KF/PE,CF/PTFE,CF/PLLA,GF/PU Tendone /
plates and Bone
screws
CF/PEEK,CF/EPOXY,CF/PMMA,CF/PP,CF/PS,CF/PLLA,CF,PLA,KF/PC,
HA/PE,PLLA/PLDLA
replacement hip CF/EPOXY,CF/C,CF/PS,CF/PEEK,CF/PTFE,CF/UHMWPE,CF/PE Total
Bonepacles/ cements PMMA,titanium/PMMA,UHMWPE/PMMA,GF/PMMA, Bone
CF/PMMA,KF/PMMA,bioglass/Bis-GMA
replacement Knee CF/UHMWPE
Hydroxyapetite
of (HA, Ca10 2) because synthetic to (PO4)6(OH) bone similarity Using hydroxyapetite appetite
20 was since interest 2]. years case of the
- - 16
coating great powder form total in used ass of biocompatibility in It hip and layer replacement. is the has
in [1] orthopaedic of 2-2: Application Figure composite polymeric
in replacements: bone of The types 2.3 composites advanced
are investigation. under that many composites are still made or are polymer There
bioactive first (high the bioethylene) 1. HA/HDPE density [2] composite
as matrix: Advantages polyethylene of
is a biocompatible and orthopedic Is it very liner in and used HDPE polymer.
reinforced apetite Hydroxy polysulfurHA/PSU 2.
is almost 40%HA. PSU Is polymer high composite with new replacement with a bone for
has bearing prosthesis[2]. It modulus better properties It mechanical strength. in load and applied is
and is than oxidation resistant and hydrolysis. to HDPE
cements Bone
Boneparticles/PMMA,
titanium/PMMA
replacement Total hip
CF/EPOXY
CF/C,CF/PS
plates& Bone
screws
CF/PEEK,CF/EPOXY
CF/PMMA,CF/PP
Intramedullary
nails
CF/LCP
CF/PEEK,
GF/PEEK
Polymeric
composite
orthopedic in
- 17 -
3. high Bioglass reinforced polyethylene density
To bone improve bonding be between to found increase are and better reaction implant, and glasses
and than Composites HA. bioactive volume. 30% bioglass are made with more
4. phosphate polyhydroxybutyrate reinforced Calcium copolymer its and
- composites PHB TCP/ PHB. [2]. and polyester biodegradable is liner -hydroxyacid are
5. Calcium chitin phosphate reinforced
Chitin is PcHA/ and biodegradable also polymer natural chitin.
6. Bioactive scaffolds: and biodegradable
and the Bioactive Chitin biodegradable have poly(L-lactic acid) or matrix (PLLA)as scaffolds
polymer psHA/PLLA[2]. and containing HA, while 20%bioactive ceramic
2.4 materials: Advantages polymeric of composite
• low strength and High modulus.
changing it fraction reinforcement/ of to and phase the matrix design By is • possible altering
make physically for and different mechanically and tissues. implants the suitable
There like metal corrosion implants. no • in is
and X-ray are in totally some • not failures Metals show radio can radiography ceramics and
polymeric transparent But of can composites material transparent. help some the by be contrast
to the polymer.
composite shown Polymeric with materials have diagnosis • many new compatibility high
MRI because not as as computed well like: magnetic they methods are tomography(CT).
composites Reinforced fatigue un-reinforced resistance composites, than • more have
very which joint knee is in replacement. important
- 18 -
Structural 3. composites reinforced Material in
Polymeric 3.1 phase: matrix Materials as
3.1.1 polymers: Thermoplastic
they (due form moisture and strong show wetting to and to bonds, are biocompatible - resistance
bonds) [4] strong (PEEK-PAEK)
3.1.2 polymers: Thermosetting
they biocompatibility different are durability. in as They vary Epoxy Such and - are resins, and
applications. found in not in they good so fracture orthopeadic attractive to fixation. be have But
is better thermoplastics Their characterization much processing than [4].
Resorbable materials 3.1.3
fracture in support To materials the used more, be reinforcing material fixation must sometimes
PLLA like also that a should matrix fibers, PLLA/PLLA to be resorbable composite which of leads
[4].
Carbon/ 3.1.4 carbon composites
shortcoming biocompatible. the are - possible to carbon released the that are is But very particles be
the in tissue [4].
Ceramic 3.1.5 composites. matrix
and They well biological include properties titania as as have zirconia- good Hydroxylapetite-
have alumina, resistance[4]. but low they fracture
as phase: 3.2 Material Reinforcement
Fibers Particles
filament Particles 3-1: Glass 3-2: [8] fiber Figure Figure [7]
- 19 -
Reinforcing material in composite can be used in 2 forms: Fibers and Particles (Fig. 3-1 and 3-2).
Role:
They give more strength to the matrix but the reactions between matrix and reinforcement is different
depending on the type of materials
3.3 Reinforcing material in orthopedic composites:
3.3.1 Carbon fibers
Figure 3-3: Carbon fibers
- are popular and chemically biocompatible with human tissue. In the form of composite, carbon
fibers can have good strength and stiffness.
They can be used in different forms:
-Long and unidirectional fibers-(they have more strength and stiffness)
-Short and chopped fibers (lower strength)
-Woven fabrics that have medium strength. [4]
3.3.2 Glass fibers
They have Strong mechanical properties and are relatively cheap. They have high Tensile and
flexural strength; they have good temperature resistance and fatigue resistance
Figure 3-4: Glass fibers [9]
-20 -
Bioglass: 3.3.3
[10] Figure Bioglass 3-5:
and in water, They to and It recently properties. are found have is out developed not good solving
so durability in body[4]. can long the offer they
Aramid Kevlar® 3.3.4 fibers as: such
Figure Kevlar® [11] 3-6:
high properties, Kevlar low strong and it so offers but not is compression stiffness tensile and
in popular orthopedic applications[4].
process composites 4. of Fabrication orthopedic
according well selected as as the and material technique processing be should The to the design
of the composite. application
be manufacturing: The following considered in factors should
device and of 4.1 Design material the
from we composite. should properties considered development which sample our It expect be The
the some the bases for sample of is necessary. of theoretical design
implantable 4.1.1 composites: aspects of Biological
Both matrix a interaction Biocompatibility and of is reinforcement implant tissue. and between result
biocompatible. be biologically should
- 21 -
composite: of aspects implantable Mechanical 4.1.2
test enough by some high It should be durability which evaluated strength, and enough can have
methods[4].
4.1.2.1 Strength orthopedic of composite:
are natural than to means stronger that It strong. normally Composites be required they should be
because bone than section less cross of implant but dose the implant the of also tissue has; bone
repair the to The composites is like fatigue. of the ability related to have damages strength the not
and the fibers reinforcements the volume the direction fiber of and also length of
4.1.2.2 Durability:
have durability. Orthopedic has composites it desired long seen in composite materials But to are
of they of observed. breakage have matrix-fiber Some that was some cracking after period time. fatigue
the composite[4]. It also on on stress applied depends
Processing methods 4.2
composite on manufacturing are depending methods for There different production, used matrix
the has and reinforcements, composite shape, desired different and application to be made.
Hand lay-up 1-
moulding or vacuum 2- Vacuum bag bagging
injection Vacuum moulding 3-
transfer Resin moulding 4-
Compression 5- moulding
lay Hand 4.2.1 up:
has procedure The following steps:
in mould sealing of is made - size tapes The samples prepared. special
is layer resin of mould. A - the applied on
woven glass or fibres it. The - on are placed
the - bubbles or brush process). (milking Manipulating to air remove roller by
fibbers By impregnated glass pressure inside by - plates are glass using applying resin with the
mould. the
22 - -
of are Depending sample, layers mat or desired of the on - added. fibbers more thickness
rollers using of by - airbubbles, and Removing milking.
top of is placed - film the on sample[6]. Protective
cured (heat) result resin using and or is curing and hard room temperature by in methods At -
sample. brittle
low sample to is strength of normally quite of due ratio this technique the high the With •
reinforcement. resin/
because amount In so would not up prevent can of the enough hand be lay resin low • it
in of the resin[5]. soak fibres
thin This in samples method results • large composite. and
and time lot good is consuming, • It careful needs quality skill control[4]. and a of
of Figure Preparation woven and 4-2: 4-1
and Figure resin milking of by [12] apply Impregnation 4-4: 4-3: Resin fibers Figure
- - 23
[13] technique Figure lay-up 4-5: Hand
moulding: Compression 4.2.2
to the this placed In and film) resin is material (reinforcement, protective the method moulding
65º adjusted a a material depending is (in test machine C), the on certain and our , temperature
closed. mould applied 30 kN) (our the is and certain After 3-4 case and pressure pressed is then
the is removed minutes from and the machine. cured sample our preliminary in test
machine: Compression moulding 4.2.2.1
machine: of the Main parts
parts Matched 1- moulds
Heater 2-
force Some 3- devices to create
be: The for moulds can compression
moulds - Hand
process are and used mould moulds: for loading; of -Automatic automatic press other the part and
are automatically controlled.
- Semiautomatic the is moulds: remove from the an material load and needed to operator part
the mould.
For used experiments are hand moulds [5]. our
- - 24
Figure [14] 4-6: Compression moulding
4.2.3 technique: bagging Vacuum
the fibre glass of strength In glass resin that and made increases resin, and are fibre composites
the supply manufacturing of weight. desired resin Less amount in methods. increases is
this the or to pressure (from fibers the is resin above squeeze surface) In and method used and
the of the the system out rest and pushes of system. flattens resin
Procedure:
system by fibres covered by resin and is contains impregnated -The a film protective (releasing
that preferably to stick film) resin. porous to to the is prevent
is turned vacuum system -The the on is the to inside removed pump air and the vacuum and due
pressure (pressure strongly on change sample. the the film the to attach drop), starts in surface of
leads This the flowing extra is further to the out sides. to resin that
of -Primarily in for hand some curing Afterwards, by machine curing sample seconds. curing the
flash, ended) (Hera is process Photopol [6] ovens the curing
4-7: rulers Laying using [15] the by Figure fibers
- - 25
Resin Injection moulding 4.2.4
of this process: Steps
are shape is what and the to preformed designed according - The (reinforcements) to woven desired
for form, composite. of sandwich and example composite, size the for the
Applying resin mould. the the to -
- Preliminary curing
Removing - the sample
- Final curing
lower thermoset commonly The are method. with RTM used in more resin viscosity
starts pressure, laminate Because flow At resin sample). (mould this the the contains in to of
the flow resin it help before would be It resin better the injection. stage to will preheat to mould
this (lower resin easily. viscosity is The more pressure related flow of to resin the and in part
in flow). resin viscosity higher a results
the performed. resin After fibres impregnated [5] curing is
Advantages:
needed manufacturing forces work are during costs. process less -Less
parts made be and by this using shaped can technique. -More complex different
Disadvantages:
can residuals interesting. this - be that are not much process produced In
cost of [6] - High equipments.
the calculate resin: is With filling/ time the sample to it impregnation by possible Law of Dracy’s
Time:
p k
l
2
2
500MPa´s Is flow 100 resin of the viscosity: directly can normally time of Resin in be and range - the
resin above. equation viscosity to of related according the to
and permeability: porosity Reinforcement
between 0.85. reinforcements is 0.5 The porosity - of used permeability the But in composite most
affected size, flow be by can be sample different. time shape. and volume can also The
26 - -
pressure: Applied
pressure is less applied mbar. the than flow, To 100 the best resin achieve
sample from In there comes pressure and pressure transfer inlet is moulding of higher resin the the
side. inlet in [17]
injection Vacuum 4.2.5 moulding:
moulding applied for which method, a moulding method can This be closed method open and is
covered upside of a by film. the method where the sample is
flows this resin bagged with the help of the vacuum pressure method In through the laminate.
(in for and in is of one or applied case sides on One more sample the resin down our entrance
side resin side entrance. is one sample) in outlet vacuum the of opposite for situated of the
100mb) performed By the is pump, vacuum supplied the gradient inside than (less a pressure using
and reinforcements. sample the flow the causes through resin to impregnate laminate and
at cure) end, After pressure same impregnation hand the and laminate cured (preliminary the is the at
in then curing and oven. continued is
process: of the 4.2.5.1 Steps
plates: Aluminium a.)
warm used the heating oven to process after , sample keep up the them in during (for are they
flow). better resin
tape: b.) Sealing
sample. tapes According and for size, form form used are to It sample to make sealing a helps
sample. and and the inlet This protective also coating adhesion films tubes material on outlet the of
wide. form rolls the in [18] about or tapes; is 1/2 of inch
tape Figure Sealing 4-8:
- - 27
preparation: c.) Preform
side top the made of that form down well of the as tapes and Is system as film sealing on contains
sample. of sample is the and This and the made fibres. to according shape the size
Tubing: d.)
and through of the sides from are Tubes sample placed flow the sample on resin resin batch for
to is piece A down. to for also cm vacuuming, connected and of up warps the tubes 3-5 spiral
help can of flow Vinyl Resin Teflon: through made tubes resin be flow mates. or flow
Thick Polyurethane LB.k2 SMCTU0805 8×5 tube:
Thin TU0425 tube: 4×2.5 SMC Polyurethane E.oj3
These of are covers and applied tube them connected piece tape sealing The again. for one tubes
resin before should and closed be prevent resin air clamp drop pressure to flow leakage by supply
through system.
e.) mats or flow media: Flow
pieces of inlet side the mat are of side placed media flow distribution Two on or and vacuum
and sample and or directions. flow through other not the the directly resin causes to perform sample
this (In Hexcel vowen 48g/m2) layer of 1080 fiber 2 experiment glass
f.) film: Vacuum vacuum bag or
of by preparation be and After tubing sample, protective the system preform, form whole covered can
film. apply should sealing good considered bagging part or connection In to and it be this
the have sealing no to tape between and film leakage.
bagging of or elastomer. vacuum can The nylon film film made be silicon
4-9: bag [19] film Figure Vacuum
- - 28
g.) Resin supply:
drops is pressure are clamps entrance the connected the and to resin vacuum the After applied,
starts resin timer removed flowing used to total the the to thesample, flow and the through show is
marked are calculate time. After final resin speed. distances flow each time Flow certain to the
resin impregnation is finished, closed is vacuum the by in outlet is for clamps applied but inlet
air some clamps to the in it remove bubbles also closed extra prevent and by to flow is then time
difference air through The resin forces flow pressure the resin reinforcements leakage. is to the
by difference. provided pressure
h.) Finishing:
sample 10 hand impregnation, end for of second is is preliminary the cured then At the and it
other curing. steps with continued [5] of
vacuum moulding injection 4.2.5.2 Why techniques?
less to hand-lay is other This • like expensive methods up. compared method
sample due (more of to mechanical • content are high fibre than The properties increased
method this achieved and content. void less 60%) by possibly
(covered system to less to and lead • mould) a closed components Due volatile released are
and less safety health [17] threats. more
structure 4.3 of Sandwich composite:
be of between placed fibres 2 to form layers make can In woven the sandwich of composites this
different forms. added. of can on layers thickness, fibres required Sandwich be the Depending
higher samples of without more higher weight with applying samples resin[6]. amount strength are
thermo Important bioactive mechanical make to methods in to consider composites: things
that the period glasses the specific be in considered processing should it and heat -In ceramics
which polymer results in resin of higher the oxidation during (polymer) process value is that than
they get if cold especially range, high that. don’t after temperature in
get the to material better it and to that dry sure is - Before molding avoid injection compression is
such as bubbles[2]. air formation the void
29 - -
Curing: 4.4
Preliminary in applied final 2 and curing. is curing Curing stages:
As beginning from the of increases, of started temperature is injection. Curing the resin the rate
polymer increases. the composite of and the cross part linking, changes After also curing curing
which glassy in more polymer converting has to the shape viscosity. after the gelatine to form
glass polymer of temperature passing After completed, is transition the stage, this cross-linking the
glassy temperature transition glass higher. is changed to because that result is The form polymer has
than temperature. sample more is increased
polymeric highly know It curing resins viscosity on depending is of are and important the that to
way the of the managed to be result best The in the get temperature. supply should amount heat
heat is process RTM and heat involved process. polymer transferring in this the in between The
curing during heat as [5] as the reinforcement polymer of well released
& in [21] Light-curing thermoset process 4-10: resins Figure of UV of light hardening exposure
temperature shows viscosity effect during the of curing The when that temperature the increases,
decreases. of resin
from from chemical components the raised Volatile are reactions sample.
thermoset Curing 4.4.1 of composites:
increases, curing time resin, of as size curing the of long thermoset In as the and temperature of
curing, polymer and increases. forming Cross the final also after linking the is occuring polymers
form. shape glassy changed is to [5]
- 30 -
Photopol oven curing light machine Light Figure 4-12: Figure Hand Curing 4-11:
oven Heraflash 4-13: Figure
part: Experimental Part II:
Method: and 5. Material
fibers include this to as make composite used in Materials experiment samples glass
phase. resin curing dental part reinforcement as and matrix
Reinforcements: 5.1
reinforcement. used are fibres Glass as
contains which E-glass used reinforcement composite of been glass fibre in most is and has as kind a
[23]. calcium-alumina borosilicate
- - 31
[22] Glass material used Table be 5-1: composite can reinforcement in
fiber Material Form of
reinforcement Fibre Unidirectional
Fabric Reinforces 2 in composite the direction
Chopped glass reinforcement Random strand
Glass mats reinforcement Randomly
Woven fabric glass than glass expensive –less roving strength High
Glass forms: fibers Company following Ahlstrom and woven from were and THS provided in
Prove ~760g/m2 multidirectional (THS) woven 1 ROVIPLY
Prove 1080-300g/ Bidirectional m2 Woven 2 Hexel
Prove roving -519g/ m2 bidirectional 3 Thick woven
Prove prove Woven 2 Bidirectional 4
Prove Woven 5 prove 3
Prove Woven 6 prove 4
Prove Unidirectional 7 Ahlstrom fibers R338-2400 Ahlstrom
Prove 1 Prove Figure Figure 5-2: 5-1: Figure Prove 3 5-3: 2
Prove 5-5: 5 5-4: Prove Figure 4 Figure 5-7: 7 6 Figure 5-6: Prove Figure Prove
- 32 -
5-2: Table woven Weight textiles measurement per area of
woven Fibres& Weight/ Diameter area Length Area weight
Hexel 1080-300 g/m²
0.08m with 0.077m 0.077 ×0.08=0.00616m² 1.8375g
Analytic balance
298.29 g/m²
woven 518.60 0.081m bidirectional 2.9825g 0.071m g/m² 0.071×0.081=0.005751m² Thick
fibers 4.7948 0.089m 0.071m 758.79g/m² Multidirectional 0.071m×0.089m=0.006319m²
fibers m 2.330g/m² 1.09 Unidirectional 2.54g
2, microscope of 3 observation is under structure their 4 of By following and prove information
per each cm: achieved
2 4 Prove Ahlstrom R338-300tex to
in 1 2: cm weft 9.2 bundle Warp= Prove each bundle in and = 7.2 1cm
in 8.3 and = cm Warp= 3: 1cm Prove 1 in weft bundle bundle 9.4
bundle 9 and weft 1cm Warp= 4: 1cm Prove in bundle = in 11
Resin 5.2 matrix part: or
curing matrix been based Dental dental As resin material material resin. in used we had This used
It applications of from years plastics. since the some group is thermosetting ago.
used are most glass fibre; matrix unsaturated with Nowadays, material as is reinforcements thermosetting
or resins. polyester epoxy resins
they in of or issue not crosslinking release this material volatile that do Advantage is components
polymerization [23] or reactions.
of curing Constituents resin 5.2.1 dental
TEGDMA: Tri(ethyleneglycol)dimethacrylate95% •
material for of reduction a viscosity. as Used solvent
Bis-GMA: BisphenolAglycerolate (1glycerol/phenol)dimethhacrylat •
Portion: 70%2,2-bis[4-(2-hydroxy-3-methacryloxyprop-1-oxy)propane.
has material a as sealant. been viscose and very is application used dental in It
GMAin of degree between 50-70%. Bis- polymerisation of composites The almost is
Dimethylaminoethyle • methacrylate 98%- DMAEMA:
polymerisation co-initiator, reaction radicals. participates a in forming by aminoalkyl As
33 - -
Chemical • [(bronanedione,1,7,7-trimethyl CQ:Camphorquinone: formula:
bicyclo[2.2.1]heptane-2,3-dione]
reactions. light yellow a powder polymerisation cured is in used and as It easy is initiator to be
photo reactions. and initiates the polymerisation
resin resin) 5-3 Table : of curing Constituents (dental
in resin % Material batch Portion
95% 30% TEGDMA
68-70% Bis-GMA
0.7% DMAEMA98%
0.7% 97% Camphorquinone
added viscose and mixed batch to material special First in then material the was portions. The is
(each viscose Bis-GMA material was added flask of or the Bis-GMA).
batch Procedure 5.2.2 for resin preparation:
flask - empty Weight is 1 of measured.
mixing) - (to of is 2 magnet measured. facilitate Weight
metal material mixer placed plate 3 added, mixer: of from the on Solvent is (temperature 35°C -
RPM). at 140
be 4 400g. size - to The batch around is desired
is of of the beginning is 5 solvent 70% The is which batch. 135g, resin around - added amount at
material are is is flask added, Then each stirring. Bis-GMA while the added
is added 6 Camphorquinon -
facilitate get 30 minutes of champhorquinon and oven warm for to Placed at 7 - the 45°C mixing in
powder
Mixing - 8
added. chemical is last 9 DMAEMA -
Mixing - 10
is in is decicator in poured and over applied 11 flasks the The placed plastic and resin vacuum -
degassing. night for
- - 34
Mixer Figure 5-8:
procedure. resin the with 4 this were batches made lab in
resin: 5.3 moulding of Open
methods At curing by resin was of experiment, the moulded and cured different some beginning
composites. to of the curing condition the best find for rest
co1 Resin F1-UCB-007 batch
Procedure:
measured. mould The was (Teflon) - weight PTFE of
minutes. 10 preheated 15 - was - oven Resin in for the 45ºC at
- to lab polymerisation. be initial photo the lights in should prevent The turned off
- to added mould. 11-12g the is resin About of
- a surface film air such bubble between placed the that in Protective no is trapped mould way on is
of and film. mould
- applied forms Light in is different curing
Table of different 5-4: Effect curing on conditions resin
Sample Weight Curing method
12.55g Hand sides) curing curing Heraflash preliminary & light in 30s*2(both oven F1-UCB-007-co1
min light 120ºC oven cured 2 Post (Photopol); at for 15 hour
11.47g Hand sides) curing curing Heraflash preliminary & light in 30s*2(both oven F1-UCB-007-co2
15 (Photopol) oven min light
11.62g oven Heraflash light in & curing curing Hand preliminary sides) F1-UCB-007-co3 90s*2(both
oven min(3*180s) Heraflash for Light 15
Hand in curing & light F1-UCB-007-co3 11.09g Heraflash 30s*2(both oven preliminary sides) curing
light 2 (Photopol); Post oven 45 min hour at for cured 120ºC
- - 35
Curing Reaction:
polymerization based The resin of is The of light Bis- camphorquinone basic method. curing GMA
photons the absorbs range UV of curing of 200-300 lights procedure the during nm in
of visible light range in and 400-500 the of nm. also photons
and is initiated via by The the champhorquinone photoinitiating polymerization. reaction starts
polymerization the co are initiators For The (amine) participating. are the rate, increasing radicals
from by Along the these polymerization. that start initiators exposure with formed light radicals
of the are dimethacrylate polymerized. and monomethacrylate monomers
CQ UV In like of an and the (dimethylaminomethyl presence the methacrylate) organic amine
cross at light is linking reactions starts. apply needed and absorbed to is time light The which the
stage seconds[16]. the - is about 20 40 beginning
protective to melinex connected to before be It be sample film that has still must considered the the
to can oven oxygen exposure and them placing because inhibit prevent Heraflash oxygen in
can radicals by some stop the the It forming inactivate peroxides polymerization CQ reactions.
polymerization in lower rate. which stop can reactions
and Grouping 6. samples: of Manufacturing the
named according The number. to are batch samples resin
the of Name batches: resin
F1-UCB-00x
to Refers fiber reinforced F:
college University of Borås UCB:
number 00x: batch of
of Name samples: the
F1-UCB-00x-coy
to Coy: number Refers composite y
36 - -
1: technique 6.1 Group Processing
made methods: first group using samples are The of F1-UCB-008 4 different processing by
Hand lay-up 1 -
Vacuum bagging 2 -
Compression moulding 3 -
Vacuum - injection 4
different of processing 6-1: Effect technique Table
Properties name Method Sample content Fiber
unidirectional Sandwich 1 40 Hexel F1-UCB-008-co4 fiber+
300g/m2 1080
54.07%
multidirectional F1-UCB-008-co2 layer One 2 50.72% woven
2*16 F1-UCB-008-co11 2layer of Unidirectional 58.69% bundle 3
unidirectional 4 fiber+prove4 Sandwich of F1-UCB-008-co10
bidirectional
74.63%
vs. content Figure Method 6-1 Comparison fibre
0
10
20
30
40
50
60
70
80
Fiber
content
%
4 2 1 3
Method
- - 37
results Comparison different method of
Vacuum Figure bag 6-3: 6-2: injection Figure Vacuum
Hand Figure lay-up 6-5: 6-4: molding Figure Compression
injection. vacuum is Therefore, the be 6-1, method was As obvious best to figure it found from
content fibre of (higher made higher by vacuum injection the the were of samples rest because
the in the samples. air content bubbles as well strength ample) less void and of as
structure: Wovens fibres 6.2 sandwich vs. 2: vs. Unidirectional Group
experiment: used fibre Following in and woven are
fibres Thick bidirectional -
(Hexcel) Bidirectional fibres -
fibres Multi directional -
fibres Unidirectional -
- - 38
structure different Effect 6-2: fibers sandwich Table textile vs. of woven and
Sample Form flow of name time loss Resin Ignition reinforcement
F1-UCB-008-C06 bidirectional 65 Thick fibers 34% min
F1-UCB-008-C10 fibers 25 Bidirectional (sandwich) 25% min
F1-UCB-010-co12 Multidirectional 28% (sandwich) 18 fibers min
F1-UCB-008-C13 Unidirectional 23% fibers 70 min
Sandwich structures:
form on consists core woven textile a both and This the of (usually material) of composite light
Normally the structures higher facilitate resin The layers woven sides. have sandwich stiffness.
flow sample. the through [24]
ratio structures weight to strength in stiffness The of high. [25] is or sandwich
Figure structure Sandwich 6-6: [26]
Figure structure 2 Sandwich 6-7:
Film
Woven
Fiber
- 39 -
stage some the form At fibers of different experiment compared glass are of samples this made of
and characterised.
6-8: Figure UCB 008-C13 F1
6-9: Figure F1-UCB-008-C10 6-10: Figure F1-UCB-008-C06
(Middle) (Beginning)
Figure 6-11: F1-UCB-010-co12
- - 40
3: Sandwich Comparison woven: Group samples: of 6.3 different
injection with method woven vacuum different of the samples different textiles made With are
textile the facilitate through and which can investigate support resin to thicknesses unidirectional flow
less and bubble content. air with fibers void
Sample woven thicknesses different Table 6-3: different with from
textiles of unidirectional Bundles Woven
fibers
of Bundles unidirectional
fibers
of Bundles unidirectional
fibers
woven Thick 60 bidirectional 80 40
300 Hexcel 40 Bidirectional 80 g/m2 1080 60
40 Multidirectional 80 woven 60
Sample groups:
applied The 6-4: injection is table shown process result and in is the vacuum
Effect woven 6-4: Table different of
flow content name Sample time Fiber Resin
Sandwich bidirectional F1-UCB-010-co10 unidirectional+thick
fiber (80)
12min 74.8%
Sandwich F1-UCB-011-C01 undirectionali+multidirectional
fibers(80)
74.7% 24min
(80) unidirectional+hexcel F1-UCB-011-C04 29min Sandwich 66.1%
Figure 6-12: F1-UCB-010-co10 6-13: F1-UCB-011-C01 Figure
41 - -
6-14: Figure F1-UCB-011-C04
Room Group Temperature Temperature: 4: 6.4 Processing vs. 60ºC
the as Some and resin as well different time were made in temperatures processing samples flow
(void measured: the bubbles content) was air amount of
of temperature Table Effect 6-5:
flow Ignition name Resin Sample temperature loss time Sample Nr.
70 77 F1-UCB-009-C01 Temp:23°C S min % Room 4-1
min 25 38 60°C 4-2 S % F1-UCB-009-C03
min 30 33 65°C 4-3 S % F1-UCB-009-C04
min 10 37 65°C 4-4 S % F1-UCB-009-C05
Samples: Processed
S S Figure Figure 6-18:S 4-3 6-16: S 6-15: 4-1 Figure Figure 4-4 4-2 6-17:
- - 42
sample Group5: Effect thickness: 6.5 of
unidirectional thicknesses bundles in different and (different layers) Samples the fibers of with
presented 60, and 6-6 results (40, 80) the were are made and compared in table core
sample Table thickness of Effect 6-6:
material Sample Sandwich Core:unidirectio Sample Nr. code
R338-2400 nal
Fiber time Thickness Wetting
content
5-1 S
5-2 S
F1-UCB-010-C07
F1-UCB-010-C11
g/m2 Bidirectional800
g/m2 Bidirectional800
bundles 40
bundles 80
mm 2
mm 3
min 14
min 26
73%
% 75
5-3 S
5-4 S
F1-UCB-010-C12
F1-UCB-011-C01
Multidirectional
Multidirectional
40 bundles
80 bundles
2.5 mm
3.5 mm
18 min
24 min
72 %
75 %
S 5-5
S 5-6
F1-UCB-011-C04
F1-UCB-011-C05
Hexcel 1080 g/m2 300
Hexcel 1080 g/m2 300
40 bundles
80 bundles
2.5 mm
3.2 mm
53 min
29 *(PA) min
66 %
55 %
Processed Samples:
6-19: 6-20: 5-2 S 5-1 Figure S Figure
Figure 5-4 5-3 Figure 6-21: S Figure 5-6 S S Figure 5-5 6-24: 6-22: S 6-23:
- 43 -
Group6: of 6.6. Effect mould size:
the group with this were In different samples made sizes. mould
Same - as 1 size mould the sample
than size the Bigger place - sample mould 2 resin to free that around can flow sample (with remove
air bubbles.)
compared The 6-7: were in shown and are results Table
Effect size 6-7: of Table different mold
size content name Mould Resin flow Sample Fiber time
F1-UCB-010-co7
F1-UCB-010-co8
mould size Bigger
mould as size Same sample
14min
21min
73.8%
78.1%
F1-UCB-010-CO10
F1-UCB-010-CO11
mould Bigger size
size Same as sample mould
12min
26min
74.88%
75%
Figure Figure F1-UCB-010-co7 F1-UCB-010-co8 6-25: 6-26:
(Beginning) (Middle)
6-27: F1-UCB-010-CO10 Figure
44 - -
(Middle) (Beginning)
6-28: F1-UCB-010-CO11 Figure
Characterization: 7.
evaluation includes Performance: of of composites Composite The the characterization
fiber/matrix morphology, arrangement Matrix •
strength, (flexural content) fibre Mechanical behaviour glass •
and content: void methods. experimentally. Residual microscope visually: by Test •
Density • measurement.
mechanical can observation, tests. samples chemical by visual characterized be and The
observation: 7.1 Visual
Flow 7.1.1 time: Resin
impregnation The find resin during and observed fibres of flow to time marked was the visually
through the fibres. speed resin the of
the Depending different. on certain for textiles, rates flow different are directions a of pressure woven
well is affects thickness affecting the part The but as speed flow the of also the sample it of resin
higher, the sample. permeability of of As on are thickness the and the layers permeability
lower. is sample the
- 45 -
0
0,5
1
1,5
2
2,5
3
23 3 16 7 12 20 14 29 1 6 25 2 8 5 18 10 4
08-co13-unidirectional Figure Figure 008-co10-prove4 7-2: 7-1:
in 7-3: flow bundle and 29min 011-co2-40 speed Figure
[cm/min] v
0
0,5
1
1,5
2
2,5
3
25 10 0 20 5 15
speed time
speed 011-co1-multidirectional Figure flow 7-4: with
- 46 -
The presents from The woven that result is resin different fibres. graph flow speed and of samples
the has with bidirectional prove4 impregnation in the flow best and sandwich resin structures
woven.
7.1.2 Air appearance: bubble
composite increase samples possible as to content less void The bubbles desired as to have and are air
strength distance the distribution mechanical their The improve properties. and and amount,
appearance visual were withmicroscope. measured observation air marked bubbles and of by of
Figure End F1-UCB-011-co3 Middle Beginning 7-5:
Air 0-1-2-3-4 bubble Coding:
bubble beginning the Air 1.5 from appearance: sample of cm
Figure middle Begining 7-6: F1-UCB-011-co11
Air Coding: 0-1-2-3-4 bubble
bubble from Air appearance of 3cm beginning the sample
0
1
2
3
4
0
1
2
3
3
4
- - 47
Tooling samples: of 7.1.3 the
the observed sawing sample edges: in machine, were edges by cutting After Cutting the microscope
there the also is of if and to fibre/reinforcement see arrangement. estimate and fibres frying
F1-UCB-010-co12: uni after multidirectional + 7-7: Figure polishing
F1-UCB-011-co5 Hexel 1080 Sandwich bidirectional 7-8: Figure 300g/m2+unidirectional
7-9 F1-UCB-009-co3- Figure R338-2400 Ahlstrom
shown in good 7-9 left Not fiber/matrix Figure the on arrangementis
7-10: Figure machine Sawing
Thickness measurement:
in was from the measured of sample. different the thickness distances The sample beginning
48 - -
Chemical 7.2. tests:
samples To were chemical tests the applied. some characterize
Gravimetric (TGA) 7.2.1 Analysis Thermo
it or an the is TGA measure (loss analytical changes makes possible method to which weight
By loose temperature. weight heating, materials by gain) of can some a but applying material
a with as surrounding result of gain other materials reaction environment. can weight
temperature on chemical in reactions as a change weight result of reactions is critical different The
design suitable in adjustment reactions. analysis is thermal and necessary to thermal
of material, and oxidation re-hydration. in are structural Applications decomposition sulfur
where of shown are graph gain are percent as or of results the The weithgt weight a TGA, loss
content to this comparison. used a In fiber experiment [%] in [27] determine shown. as cent we per
TGA Figure machine 7-11:
Procedure 7.2.1.1.
pieces representative 10-30 samples were cut between mg. and chosen small in weight at Some a
were samples homogenous were grinded cutting have distribution edges The and sides to applied on
the of sample. fibres in
Samples: 7.2.1.2.
samples: Selected
samples, samples - High 2 parallel content: 1 fibre 3
sample, 2 content: - parallel fibre Medium 2 3
sample, 2 content: - parallel fibre Low 3 3
6 samples = selected were of parallel tested: 3 From * each samples are 3 18.
- 49 -
of the curves. are represented results in form The TGA
vs. a content as TGA low Fibre method: ignition method fibre comparison loss 7-1: Table measurement
samples content
loss Sample content Fibre Fibre /ignition content name method /TGA
750c Temperature Temperature 650c
62.25% F1_UCB-008-Co3 53.38% 45.11%
TGA Table fibre comparison ignition Fibre medium measurement method 7-2: vs. method: a loss as content
samples content
/TGA Sample method /ignition loss name content Fiber Fiber content
800c Temperature Temperature 650c
54.86% - F1_UCB-008-co2 50.72%
67.35% 65.08% F1-UCB-011-co5 55.4%
method: method ignition loss measurement a vs. comparison TGA Fibre as Table 7-3: content high fibre
samples content
method /ignition /TGA Fiber loss Sample Fiber content content name
800c 600c Temperature Temperature
74.58% 75.21% 78.20% F1_UCB-010-co9
68.10% 77.45% F1-UCB-009-co1 70.84%
F1-UCB-009-co1 Figure 7-12:
- - 50
F1_UCB-010-co9 Figure 7-13:
Tests 7.3. Mechanical
measurement: Fiber Ignition loss content/ 7.3.1.
This method is method it based Loss or Ignition on combustion content. of resin matrix With the
is possible to [29]. D-2584-02 measure ASTM by method: Fiber content Standard in% using Test
The fibers heat measured. in weight the the resin and the burned is by furan is remaining out of
7.3.1.1. Equipment:
Figure 7-15: Figure 7-14: Electric (about ml) Furan Crucible 30
7.3.1.2. samples: Test
Selected with cut composite sawing had be machine. samples to
size weight The the sample: g is of 25mm* 25mm; between: 3 - 5 the
using get By sawing machine removed. and the the cutting smooth the frayed is area edges
The should be sample homogeneous.
- 51 -
7.3.1.3. Procedure:
are placed Then 565° and C crucibles 30 at the - minutes. put in for they are The furan removed
to get crucible cold measured. at desiccators The room temperature. to is weight
samples - The crucible the sample test of to and the are weight measure weight put in crucible
containing Then the on the stops. crucible left ignited burning to sample and flame burn is until
on in to ignite after 7-17: crucible ignition Sample Figure Sample flame 7-16: Figure
specimen Then in the about 565°C they are and at 4 furan are for hours. placed The crucible -
get at room cooled removed to temperature. in desiccators
this is weight stage, After the measured.
Measurements calculations: and 7.3.1.4.
Weight of 1) crucible
Weight of 2) sample
Weight sample 3) and crucible of
of sample and after ignition Weight 4) crucible
of sample crucible minus crucible before weight ignition and weight 5) loss= sample Weight of
after ignition
%= Ignition sample weight loss 6) loss/ *100 of weight
Loss 7-4: – 2584 Ignition Table (ASTM 02) D
(sample) loss name loss [g] weight weight Sample weight % (ignited) [g] [g] [g] weight (crucible)
5,1536 25,3% F1-UCB-011-C01 1,3040 33,5157 29,6661
5,7940 33,9% 29,9424 1,9617 F1-UCB-011-C04 33,7747
3,2222 44,6% 28,4146 1,4356 F1-UCB-011-C05 30,2012
of ideal content are this some 60-70% method samples selected the fiber With were determined,
fiber content.
52 - -
Void 7.3.2. content:
measure by content D-2734[28]. ASTM Standard using was Test method: composites % of Void
which suitable composites This for ignition lost the and those is test is density determined, method
should the also of samples be known.
densities is 2 method determined The difference based methods the by are on (theoretical in which
higher measured less and led density before, density). quality said to content As of the void
worse the properties. sample mechanical and
Procedure: 7.3.2.1.
composite calculated - Density of is
be: experiments literature glass to fibers - 2.54g/cm3; wer assumed in they our of from Density
- g/cm3 0.9 between 13.5
of density: Calculation 7.3.2.2. Theoretical
) 100(
f
r
D
R
= T +
Theoretical T: density
Density D: Resin
in Weight% resin of composite R:
in r: composite content% Fiber
density d: Fibers
content 7.3.2.3. measurement: Void
2 methods: Can calculated by be
1: method - Test
d
d d
T
M T
V
−
100 =
[%] void content V:
composite Theoretical Td: of density
volume (by Measured hand or pcnometer method) Md: density
- - 53
2: - method Test
content theoretical calculated, void this method aim is not density With the just the measurement. is
) 100 (
g r
d d
g
d
r
+ M = V −
density Measured Md:
resin of Weight% r:
g: of reinforcement Weight %
dr: density Resin
dg: density Reinforcement
Some composites sample were selected:
- samples quality (with High air bubbles) less
- (with samples bad Low of bubbles) lot air a
The of the selected measured - is result in the was represented content and void tables: samples
Table 7-5: samples) high quality content void (low with Samples
Sample Fibre content Density Void content
F1-UCB-013+014-co2 75.57% 13.5-13.8 TGA 1.73
F1-UCB-013+014-co3 8.6-8.8 73.86% 1.8
F1-UCB-010-co13 9.2-9.4 74% TGA 1.8
F1-UCB-011-co7 9.7-9.8 78.03 TGA 1.85
F1-UCB-010-co11 7-7.2 1.85 75%
7-6: content void low (good samples) Table Samples with
Sample Void Density content content Fiber
F1-UCB-013+014-co1 2.01 2.4-2.7 TGA 78.83%
F1-UCB-008-co5 1.75 1.1-0.9 58.59%
F1-UCB-008-co10 1.9 74.63% 3.5-3.9
7.3.3. Density
of is samples and by the method. hand The Pycnometer determined volume density
- 54 -
7.3.3.1. Pycnometer method:
is possible it can in the accurate. be using it As to seen very determine Pycnometer the By density
a picture, the a bottle a cap is glass hole. or capillary that Pycnometer contains flask with
Density • of resin: liquid
Procedure:
is water. filled distilled by 1-pycnometer
Volume water: of
V
m
=
of pycnometer: Weight empty 31.1590g
51.878 (presented Volume of or shown pycnometer: pycnometer) cm3 on
mpycnometer+H2O 82.5933 mH2O = - 31.1590 mpycnometer = - 51.4343g =
0.99777= =51.4343/ 51.5492 VH2O cm3
H2O 22°C Temperature table water: literature from =0.99777 g/ cm3 of
and filled of is liquid resin the 2-pycnometer then by The measured. weight resin is the
mresin+pycnometer mpycnometer - mR= = 57.4501g 88.6091= - 31.1590
Resin= -V mR/ R
of From combination formula and for water V of resin:
* R = mH2O 0.99777= H2O=57.4501/51.4343 * mR/ 1.1144g/cm3
liquid 1.1144 density procedure, By this was determined resin to g/cm3 using the be: of
and Pycnometer solid of • Density composites by [20] resin
homogeneous liquid used are which for samples the are this chosen the experiment and purpose, For
(in experiment water solvent for is not this samples should be used).
hole Capillary
55 - -
Procedure:
which parts - small the in Samples 1 placed pycnometer. be cut can are in
filled pycnometer volume by 1/3 About parts. of sample solid is
samples of pycnometer and - 2 ms Weight + =mp
(the is water of rest of out fill pycnometer - empty the Water volume to capillary of 3 added comes
mH2O= hole (mH2O+mp+ms)-(mp+ms) pycnometer): of
the - water: of VH2O=mH2O/H2O Volume 4
distilled 5 Volume water - pycnometer as by until much water of filled is pycnometer: Empty
water runs from is out the by dried filter of paper. capillary rest and hole
Empty – of Vs=V solid VH2O Volume pycnometer sample: 6 -
solid s=ms/vs Density of - sample: 7
should measurement be homogeneous density used selected The . samples for and
volume Hand by method: measurement Density 7.3.3.2.
of weight 3 about 5 this in The - are at regular with cut samples g. forms method a
thickness) measured The the the samples of are volume height/ - and (width, length dimensions and
length = the * sample is calculated width height * of
is weight of measured. the sample - The
ms/ of sample vs = - Density
is samples, presented For selected methods in and the density the is result the both by measured
1.7-2 The between tables. density is g/cm3 Samples of
2 Some methods: tables as between comparison
volume method: 7-7: Table comparison measurement: method/ hand Density pycnometer
volume Density/Hand Sample Name Density /pycnometer
1.722g/cm3 1.937g/cm3 F1-UCB-010-co12
1.949g/cm3 1.875g/cm3 F1-UCB-010-co7
1.935g/cm3 1.971g/cm3 F1-UCB-010-co8
1.990g/cm3 1.853g/cm3 F1-UCB-011-co5
2.188g/cm3 1.79g/cm3 F1-UCB-010-co10
2g/cm3 1.928g/cm3 F1-UCB-011-co10
- - 56
method based Sample tables manufacturing on
injection 7-8: Table Vacuum
time result density Fiber Sample Flow Visual content content Void
1:05 F1-UCB_008-CO6 65.82
1:48 F1-UCB_008-CO7 76.75
F1-UCB_008-CO8 75.21 3:45
F1-UCB_008-CO10 74.63 25 1.9 3.5-3.9
F1-UCB_008- 1:10 CO13 70.7
F1-UCB-009-Co1=Go1 1:10 77.45 1.7
F1-UCB-009- 1:10 Go3 62.21
F1-UCB-009- min 67.04 30 Go4
F1-UCB-009- min 63.56 10 Go5
F1-UCB-010-Co7 14 1.9 73.4
F1-UCB-010-Co8 3.9 21 TGA 1.93-1.97 78.01
F1-UCB-010-Co9 27 75.21
F1-UCB-010-Co10 12 74.88
F1-UCB-010-Co11 1.85 75 26 7-7.27%
F1-UCB-010-Co12 1.6-1.8 71.7 18
F1-UCB-010-Co13 1.8 9.4-9.2 22 74%-TGA
F1-UCB-011-Co1 74.7 24
F1-UCB-011-Co4 66.1 29
F1-UCB-011-Co5 55.4 53 1.85p-1.9
F1-UCB-011-Co7 78%-TGA 34 9.7-9.8 1.85
F1-UCB-011-Co8 34
F1-UCB-013+014-co1 2.4-2.7% 78%-TGA 2.09
F1-UCB-013+014-co2 13.5-13.8% 75.57-TGA 1.73
bubbles 8.6-8.8 Air 1.8 from 73.86% cm F1-UCB-013+014-co3 4.5
7-9: bagging Vacuum Table
Visual Fiber bubble content result-Air appearance Sample
F1-UCB_008-CO2 50.72
F1-UCB_008-CO3 45.11
- - 57
Hand up sandwich Table 7-10: lay technique-
result content Visual Sample density content Fiber Void
F1-UCB_008- co4 54.07
58.59% F1-UCB_008-CO5 0.9-1.1 1.75
7-11: Compression moulding Table technique
result Visual content Sample Thickness Fiber
C011 F1-UCB_008- 58.69
F1-UCB_008-CO12
8. Results
thesis, conditions of this composite different and of During lot part a practical the samples in
had made. processing factor been
step some each in From from representative were all samples group, prepared each and samples
mechanical best achieve chemical selected to properties the and by the characterized and tests of
composite samples.
analyses not be some work, boundaries carried of to to Because out need could be and this thesis
strength Fatigue mechanical as: such on resistance worked future the in to evaluate Tensile and
of properties and the sample. strength
during been has experiment as summarised done of results can the The following: be what
2 curing F1-UCB-007-co2) (F1-UCB-007-co1, the the resin, samples For • curing, after first
light not But yellow. much yellow changed in was colour (F1- 3rd to sample the the from
in it UCB-007-co3) after the polymerised better curing a observed. and change was colour was
than • Better fibres unidirectional impregnation with and structures unidirectional woven with
resin easier be flow fibres, resin impregnation). and to to by time which found wet was (less difficult
vacuum higher technique moulding • injection fibre with processing found to be The best has
better properties in the content which of and also less content mechanical sample. results void
58 - -
out Hexel found fibre reinforcing material, bidirectional Within it the • that have was used
impregnate are shown with resin better easier phase and by matrix arrangement to less with
bubbles. air
resin - 65ºC) been higher shorter impregnation and better (60 has flow In • temperature time
room compared with temperature. observed
material, using matrix • resin and fibres complex based With polymer more glass composites
and medical manufacture like impregnate are possible with to Implantable devices low
Voids. amount of
light • The method can materials offer flexible rigid weight but
than • Better impregnation with fibres. woven structures unidirectional
by resin. fibres • difficult to Unidirectional wet
of thicker processing With and structures, • temperature manufacturing sandwich high composites
injection resin with is moulding. possible
with possible to assumed impregnate that a even are • more It complex satisfactory is composites
voids of amount low
mould with Results samples of size bigger
resin - • air bubbles flow regular no Less
better helps to box some space leave arrangement. for Bigger • sealing
Result:
with morphology observed was the be to structure unidirectional fiber The /matrix sandwich best
4. and and 1080 fiber Hexel 300g/m2 prove
TGA Result for
Because The loss accurate a fibre seem to content. to ignition method more the method be measure
matrix of sample and more fibre which is and distribution bigger the homogeneous of size,
which represent of TGA specimen small whole sample. (10-30mg) are that for tests very the But
sample homogeneous not represent can
- 59 -
References:
[1] of polymer-composite applications S., Mayer a ‘Biomedical Ramakrishna J., materials: 2001,
review’, pp. - 61, Science and 1224 Vol. Composite Technology, 1189
[2] composite Wang, tissue materials replacement’, for Biomaterials, Min bioactive 2003, ‘Developing
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Liu 2007, composite tissue [3] a for Y., M, material bone Current ‘Developing repair’, Wang.
Applied Vol. - 554 7, Physics, pp. 547
S.L.Evans, P.J.Gregson, orthopaedic implants’, ‘Composite [4] technology 1997, in load-bearing
Biomaterials, Vol. 19, 1342 - 1329 pp.
Adams, [5] Frederick materials”, advanced of (2002) characterization Donald composite “Experimental
Third edition, University USA Akron, of
Brent Brigham Materials [6] Strong, and (2006) Edition, “Plastics: Processing”, Young Third A.
University
http://www.kissolar.com/images/fiber%203mm%202.jpg Company” (consulted [7] “kissolar (2009),
November 2008)
http://www.fiberglass-china.com/products/20057614541822.jpg (2004), [8] “CHINA YANGZHOU
FIBERGLASS (consulted GUOTAI Co.Ltd” November 2008)
http://www.rtpcompany.com/products/structural/glass.jpg (2009) “RTP [9] Company
Plastics” (consulted November Imagineering 2008)
http://www.engr.iupui.edu/~tgchu/myweb/images/bioglass_scaf.jpg [10] “Advanced (2007),
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(2009), [11] Marketplace”, “Bikudo B2B Global http://www.bikudo.com/photo_stock/48677.jpg
(consulted 2008) November
[12]http://www.dpdillon.com/cozy/tipstechniques/howtolayup/images/Cozy_chapt6_Mar07_042
a (consulted layup fiberglass Daniel “How 2008, _small.jpg, November do to by 2008) Dillon”,
(2001), Operations” “Polyester http://www.baaqmd.gov/pmt/handbook/hlayup.jpg Resin [13]
November 2008) (consulted
[14]http://www.substech.com/dokuwiki/lib/exe/fetch.php?w=&h=&cache=cache&media=compr
(Substances&Technologies)”, (2009),”SubsTech ession_molding.png November (consulted
2008)
60 - -
(2006), http://www.twi.co.ir/images/common/equipment/ksfcs002f3.jpg Ltd: TWI World [15]
Joining Materials (consulted November 2008) Centre Technology, for
(2003), R.G Missouri, Properties .Graig, Manipulation” “Dental and Materials. Powers, J.M [16]
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van Labordu Brouwer and ,D Herpt W. [17] M.

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