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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 A ril 200!

Elastic modulus of composite


" calculated #y rule$of$mi%tures " ne&lect contri#ution of matri% " ' c ( ) * + *, - . ' .
" *+ " *, " VF " '. fi#re len&th distri#ution factor fi#re orientation distri#ution factor fibre volume fraction elastic modulus of fi#re

Determining Vf is problematic
" fi#res /float0 in water " fi#res are hy&rosco ic
1 wei&ht is function of moisture content 1 !234 loss in 5ute yarn dried 306C for 70 min

" cross$sectional area of the fi#res


1 not normally round

Determination of Vf
" " " " " " " " tow countin&8areal wei&ht direct wei&hin& density &radient Archimedes rinci le resin #urn$off thermo$&ravimetric analysis chemical di&estion microsco y

Vf by tow counting areal weight


" tow countin&
1 for U9 com osites in an o en$ended mould
:rafil ;est <ethod 70222!

" fa#ric areal wei&ht


1 in a mouldin& of known thickness
CRA: method =000$2

Calculate volume fraction from fabric areal weight

" -f ( 5 A. 8 f t
15 1 A. f 1t num#er of layers of fa#ric areal wei&ht of fa#ric >k&8m2? density of fibre !"g m#$ thickness of laminate >m?

Vf by direct weighing
a closed mould is used no fi#re is lost in the mouldin& flash mass fraction after fa#rication ( mass of fi#re8mass of the com osite2 accurate densities needed to convert the mass fraction to a fi#re volume fraction2
:rafil ;est <ethod 7022=7

Vf by density gradient
o#serve the level to which the test s ecimen sinks in a column of li@uid when the density of li@uid chan&es uniformly with hei&ht2 a#sor tion of li@uid may com licate the analysis when natural fi#res are under test
:rafil ;est <ethod 70=2=2

Vf by Archimedes principle
wei&ht measurements
in air and in water a#sor tion of li@uid may com licate the analysis when natural fi#res are under test2
:rafil ;est <ethod 70=22= CRA: methods A008=000$=

Density
" density of resin ty ically ==00 k&8m 7 " density of fi#re ty ically =300 k&8m 7 resolution of B m&8cm7 for =4-f CRA: method A00 for density of .RP
1 =& or more wei&hed in air and in fluid 1 accuracy C0224 desira#le for -f and -v 1 immersion fluid at 27 C 26C

Density of %ute
" dried 306C for 70 min " wei&hed in air immediately " immersed and de&assed in fluid
$DD0 m#ar water E $B00 m#ar acetone

" wei&hed in fluid


F ( =233DC0207G in water8Hlfotol at 222!6C F ( =23B2C0207G in acetone at 20276C
data from Richard Cullen ima&e from Jean$Phili e le Iours

Vf by resin burn&off
ina ro riate for natural fi#re com osites
oven at BA0$3006C until constant wei&ht #oth com onents of the com osite will #urn CRA: method =000$7c

Vf by T'A( Thermo&'ravimetric Analysis


" ;:A measures wei&ht chan&es in a material as a function of tem erature >or time? under a controlled atmos here " rinci al uses include measurement of material thermal sta#ility J com osition2
htt E88www2tainst2com8 roducts8t&a2html

Vf by T'A( fla) fibres


" rimary decom osition eak
1 BB$D=4 wei&ht loss #etween 7=B$7326C

" secondary decom osition eak


1 2$774 wei&ht loss #etween !03$!3B6C

" ash !$D 4 #y wei&ht KSS Sharma et alE Lueens$Melfast89AIH


" ;hermochimica Acta, =DAA, =72, =0=$=0D2 " J ;e%tile Hnstitute, =DD3, AG>2?, 2!D$2BG2 " J A Polym Sci, 2000, GB, B0A$B=!2

Vf by T'A( fla) *D+E


" Pure fla%
" decom osition starts c2200$2=06C " 74 wt loss #y 7AB6C " N!006C de&radation slows >ash?

" Pure K9P'


" de&radation starts c2!=0$!706C " D4 wt loss #y !D06C
; Powell et al, 'n&ineerin& ro erties of fla% fi#er and fla% fi#er$reinforced thermo lastic in rotational mouldin&, ASA'8CSA' meetin&, Saskatchewan, Se tem#er 20022

Vf by T'A( sisal starch


hemicellulose J cellulose &lycosidic links
1 decom osition eak at 7006C

" al ha$cellulose
1 decom osition eak at 7306C

" li&nin
1 decom osition #etween 200$B006C 1 ma%imum at 7B06C
-A AlvareO and A -PO@ueO , 200!
Polymer 9e&radation and Sta#ility, A!>=?, =7$2=

Vf by chemical digestion
" sul huric acid and hydro&en ero%ide
:rafil ;est <ethod 7022B3 CRA: method =0007a

" nitric acid


CRA: method =000$7#

" different chemicals for natural fi#res Q " microwave acid di&estion #om#
Q Journal of <aterials Science +etters Q

Vf by microscopy
" o tical or electron microsco y with com uter ima&e analysis
1 for natural fi#res enhance the contrast
" olarisin& filters or stainin& techni@ues

" ima&e s littin& eye iece


1 to determine individual fi#re /diameters0
:rafil ;est <ethod =022=7

Vf by optical microscopy
" coarse olish >recommended?
" &ives #etter contrast #ut manual intervention to eliminate scratches

" fine olish


" removes scratches #ut si&nificantly lowers contrast

" mani ulate with Photosho or similar


" to o timise contrast

" analyse with Hma&eJ


htt E88rs#2info2nih2&ov8i58

,se of -mage. software

" " " "

ori&inal o tical microsco y ima&e o timise contrast in Photosho define #oundaries convert to #inary data

Vf by optical microscopy
" S'< ima&es have low contrast
1 similar chemistry of fi#re and matri%

" ;'< re aration difficult


1 sam le area too small for sensi#le statistical si&nificance

+ro and con for microscopy


" data on fi#re cross section siOe and sha e " data on fi#re clusterin&
1 can #e @uantified #y e.g. fractal dimension

" lon& re aration times " need to distin&uish at multi le scales

'eneral references
Grafil Test Methods >reference 00020B?, Courtaulds +imited, Coventry, <arch =DA02 P; Curtis, CRAG Test Methods for the Measurement of the Engineering Properties of Fibre Reinforced Plastics, Royal Aircraft 'sta#lishment ;echnical Re ort RA'$;R$AA$0=2, .e#ruary =DAA2 .J :uild and J Summerscales, <icrostructural ima&e analysis a lied to fi#re com osite materialsE a review, Com osites, =DD7, 2!>B?, 7A7$7D!2 J Summerscales >editor?, Microstructural Characterisation of FibreReinforced Composites, Woodhead Pu#lishin&, Cam#rid&e, July =DDA2 HSMI =$ABBG7$2!0$A2 CRC Press ++C, Moca Raton $ .lorida, July =DDA2 HSMI 0$A!D7$7AA2$!2 AR Clarke and CI '#erhardt, Microscop Techni!ues for Materials "cience, Woodhead Pu#lishin&, Cam#rid&e, July =DDA2 HSMI =$ABBG7$BAG$ 72 CRC Press ++C, Moca Raton $ .lorida, July =DDA2 HSMI 0$A!D7$=BB2$22

To contact me
9r John Summerscales
School of 'n&ineerin&E RRM 00A University of Plymouth 9evon P+! AAA

0=GB2227223B0 0=GB22272237A 5summerscalesS lymouth2ac2uk


htt E88www2tech2 lym2ac2uk8sme85sinfo2htm