Transcript ESF EnviroComp Warwick 200404

The Determination of the
Fibre Volume Fraction in
Natural Fibre Composites
Richard Cullen and John Summerscales
Advanced Composites Manufacturing Centre
University of Plymouth
University of Warwick, 20 April 2004
Elastic modulus of composite
• calculated by rule-of-mixtures
• neglect contribution of matrix
• Ec = ~ ηL ηO VF EF
• ηL
fibre length distribution factor
• ηO
fibre orientation distribution factor
• VF
fibre volume fraction
• EF
elastic modulus of fibre
Determining Vf is problematic
• fibres “float” in water
• fibres are hygroscopic
– weight is function of moisture content
– 4.6% loss in jute yarn dried 60°C for 30 min
• cross-sectional area of the fibres
– not normally round
Determination of Vf
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tow counting/areal weight
direct weighing
density gradient
Archimedes principle
resin burn-off
thermo-gravimetric analysis
chemical digestion
microscopy
Vf by tow counting/areal weight
• tow counting
– for UD composites in an open-ended mould
 Grafil Test Method 302.24
• fabric areal weight
– in a moulding of known thickness
 CRAG method 1000-2
Calculate volume fraction
from fabric areal weight
• V f = j AF /  f t
–j
– AF
– f
–t
number of layers of fabric
areal weight of fabric (kg/m2)
density of fibre (kg/m3)
thickness of laminate (m)
Vf by direct weighing
 a closed mould is used
 no fibre is lost in the moulding flash
 mass fraction after fabrication
= mass of fibre/mass of the composite.
 accurate densities needed to convert the
mass fraction to a fibre volume fraction.
 Grafil Test Method 302.13
Vf by density gradient
 observe the level to which the test
specimen sinks in a column of liquid when
the density of liquid changes uniformly
with height.
 absorption of liquid may complicate the
analysis when natural fibres are under test
 Grafil Test Method 301.12
Vf by Archimedes principle
 weight measurements
 in air and in water
 absorption of liquid may complicate the
analysis when natural fibres are under test.
 Grafil Test Method 301.21
 CRAG methods 800/1000-1
Density
• density of resin typically 1100 kg/m3
• density of fibre typically 1600 kg/m3
•  resolution of 5 mg/cm3 for 1%Vf
 CRAG method 800 for density of FRP
– 1g or more weighed in air and in fluid
– accuracy ±0.2% desirable for Vf and Vv
– immersion fluid at 23 ± 2°C
Density of jute
• dried 60°C for 30 min
• weighed in air immediately
• immersed and degassed in fluid
 -990 mbar water : -500 mbar acetone
• weighed in fluid
 ρ = 1.669±0.037 in water/Ilfotol at 22.4°C
 ρ = 1.652±0.037 in acetone at 20.3°C
 data from Richard Cullen
 image from Jean-Philippe le Nours
Vf by resin burn-off
 inappropriate for natural fibre composites
 oven at 580-600°C until constant weight
 both components of the composite will burn
 CRAG method 1000-3c
Vf by TGA:
Thermo-Gravimetric Analysis
• TGA measures weight changes in a
material as a function of temperature
(or time) under a controlled atmosphere
• principal uses include measurement of
material thermal stability &
composition.
 http://www.tainst.com/products/tga.html
Vf by TGA: flax fibres
• primary decomposition peak
– 55-91% weight loss between 315-362°C
• secondary decomposition peak
– 2-33% weight loss between 406-465°C
• ash 4-9 % by weight
 HSS Sharma et al: Queens-Belfast/DANI
• Thermochimica Acta, 1988, 132, 101-109.
• J Textile Institute, 1996, 87(2), 249-257.
• J App Polym Sci, 2000, 75, 508-514.
Vf by TGA: flax/HDPE
• Pure flax
• decomposition starts c.200-210°C
• 3% wt loss by 385°C
• >400°C degradation slows (ash)
• Pure HDPE
• degradation starts c.410-430°C
• 9% wt loss by 490°C
 T Powell et al, Engineering properties of
flax fiber and flax fiber-reinforced
thermoplastic in rotational moulding,
ASAE/CSAE meeting, Saskatchewan,
September 2002.
Vf by TGA: sisal/starch
 hemicellulose & cellulose glycosidic links
– decomposition peak at 300°C
• alpha-cellulose
– decomposition peak at 360°C
• lignin
– decomposition between 200-500°C
– maximum at 350°C
 VA Alvarez and A Vázquez , 2004
Polymer Degradation and Stability, 84(1), 13-21
Vf by chemical digestion
• sulphuric acid and hydrogen peroxide
 Grafil Test Method 302.56
 CRAG method 1000-3a
• nitric acid
 CRAG method 1000-3b
• different chemicals for natural fibres ?
• microwave acid digestion bomb
 ? Journal of Materials Science Letters ?
Vf by microscopy
• optical or electron microscopy
with computer image analysis
– for natural fibres enhance the contrast
• polarising filters or staining techniques
• image splitting eyepiece
– to determine individual fibre “diameters”
 Grafil Test Method 102.13
Vf by optical microscopy
• coarse polish (recommended)
• gives better contrast
but manual intervention to eliminate scratches
• fine polish
• removes scratches but significantly lowers contrast
• manipulate with Photoshop or similar
• to optimise contrast
• analyse with ImageJ
 http://rsb.info.nih.gov/ij/
Use of ImageJ software
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original optical microscopy image
optimise contrast in Photoshop
define boundaries
convert to binary data
Vf by optical microscopy
• SEM images have low contrast
– similar chemistry of fibre and matrix
• TEM preparation difficult
– sample area too small for sensible
statistical significance
Pro and con for microscopy
• data on fibre cross section size and shape
• data on fibre clustering
– can be quantified by e.g. fractal dimension
• long preparation times
• need to distinguish at multiple scales
General references
 Grafil Test Methods (reference 000.05), Courtaulds Limited, Coventry,
March 1980.
 PT Curtis, CRAG Test Methods for the Measurement of the Engineering
Properties of Fibre Reinforced Plastics, Royal Aircraft Establishment
Technical Report RAE-TR-88-012, February 1988.
 FJ Guild and J Summerscales, Microstructural image analysis applied to
fibre composite materials: a review, Composites, 1993, 24(5), 383-394.
 J Summerscales (editor), Microstructural Characterisation of FibreReinforced Composites, Woodhead Publishing, Cambridge, July 1998. ISBN
1-85573-240-8. CRC Press LLC, Boca Raton - Florida, July 1998. ISBN 08493-3882-4.
 AR Clarke and CN Eberhardt, Microscopy Techniques for Materials Science,
Woodhead Publishing, Cambridge, July 1998. ISBN 1-85573-587-3. CRC
Press LLC, Boca Raton - Florida, July 1998. ISBN 0-8493-1552-2.
To contact me

Dr John Summerscales
School of Engineering: RYB 008
University of Plymouth
Devon PL4 8AA
 01752.23.2650
 01752.23.2638
 [email protected]
 http://www.tech.plym.ac.uk/sme/jsinfo.htm