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Outline Introduction Experimental Results Conclusion
3D Characterisation of Pore Distribution in
Resin Film Infused Composites
Fabien L´eonard1
, Jasmin Stein2
, Arthur Wilkinson2
,
and Philip J. Withers1
1
Henry Moseley X-ray Imaging Facility, The University of Manchester
2
Northwest Composites Centre, The University of Manchester
Industrial Computed Tomography
September 20 th
2012 Wels, Austria
Outline Introduction Experimental Results Conclusion
Outline
1 Introduction
Overview
2 Experimental
Materials
X-ray Computed Tomography
3 Results
Void overview
Sample L (low viscosity resin)
Sample H (high viscosity resin)
Sample comparison
4 Conclusion
Outline Introduction Experimental Results Conclusion
Overview
Void assessment in composites
The properties of a composite are detrimentally affected by voids
introduced during the manufacturing process.
The common method of determining the void volume fraction is acid
digestion for carbon fibre reinforced composites and matrix burn off for
glass fibre reinforced composites.
Outline Introduction Experimental Results Conclusion
Materials
Specimen Manufacturing
Epoxy resins:
triglycidylaminophenol TGAP (Araldite MY0510, Huntsman) and
tetraglycidyl-4,4’-diaminodiphenylmethane
TGDDM (Araldite® MY721, Huntsman)
Hardener:
4,4’-diaminophenyl sulfone, DDS (Aradur 976-1, Huntsman)
Reinforcement:
unidirectional carbon fibre fabric supplied by Sigmatex
12 k carbon tows were bound with a fine glass fibre yarn (spacing of
approximately 6 mm to give a fabric of 445 g.m−2
)
Outline Introduction Experimental Results Conclusion
Materials
Specimens
Two composite panels were investigated in this study:
Panel L was made from unmodified resin (low viscosity resin)
Panel H was made from the same resin modified with
polyethersulfone, PES (Virantage VW-10300 FP, Solvay) to improve
fracture toughness (which results in a higher viscosity resin).
Each panel (approximately 5 mm thick) was cut into five 25 mm wide
strips, along the 0◦
direction.
Outline Introduction Experimental Results Conclusion
Materials
Resin film infusion
Composite laminates were manufactured by resin film infusion (RFI)
which is suitable for high viscosity resins.
Resin films were degassed at 130 ◦
C for 1 hour and then were
immediately frozen.
The laminates were cured for 2 hours at at 130 ◦
C, 165 ◦
C, and 200 ◦
C
Vacuum was applied throughout the cycle for the infusion to take place.
Outline Introduction Experimental Results Conclusion
X-ray Computed Tomography
Acquisition
Scanning was performed at the Henry Moseley X-ray Imaging Facility
on the Nikon Metrology 225/320 kV Custom Bay system:
Voxel size: 17.3 µm
Target: Cu
Voltage: 75 kV
Current: 130 µA
Filter: none
Exposure time: 2000 ms
Number of projections: 3142
Acquisition time: 1h 45’
Outline Introduction Experimental Results Conclusion
X-ray Computed Tomography
Visualisation
The visualisation software employed was Visualisation Science Group
proprietary software Avizo Fire version 7.0.1.
The voids, matrix and yarns were segmented as follows:
Outline Introduction Experimental Results Conclusion
X-ray Computed Tomography
Visualisation
The visualisation software employed was Visualisation Science Group
proprietary software Avizo Fire version 7.0.1.
The voids, matrix and yarns were segmented as follows:
Pores
[0;60]
voids only
Outline Introduction Experimental Results Conclusion
X-ray Computed Tomography
Visualisation
The visualisation software employed was Visualisation Science Group
proprietary software Avizo Fire version 7.0.1.
The voids, matrix and yarns were segmented as follows:
Pores
[0;60]
Yarns
[150;255]
binder yarn and voids
Outline Introduction Experimental Results Conclusion
X-ray Computed Tomography
Visualisation
The visualisation software employed was Visualisation Science Group
proprietary software Avizo Fire version 7.0.1.
The voids, matrix and yarns were segmented as follows:
Pores
[0;60]
Composite
[60;150]
Yarns
[150;255]
all labels y
Outline Introduction Experimental Results Conclusion
X-ray Computed Tomography
Visualisation
The porosity distribution measurements in 3D are focussed on the
position of the voids relative to both the edges of the panel and the yarns.
The void-to-yarn distance and the void-to-edge distance can be obtained
from Avizo by combining the distance maps with the thresholded voids.
raw 2D slicep
Outline Introduction Experimental Results Conclusion
X-ray Computed Tomography
Visualisation
The porosity distribution measurements in 3D are focussed on the
position of the voids relative to both the edges of the panel and the yarns.
The void-to-yarn distance and the void-to-edge distance can be obtained
from Avizo by combining the distance maps with the thresholded voids.
raw 2D slicep
segmented voids
Outline Introduction Experimental Results Conclusion
X-ray Computed Tomography
Visualisation
The porosity distribution measurements in 3D are focussed on the
position of the voids relative to both the edges of the panel and the yarns.
The void-to-yarn distance and the void-to-edge distance can be obtained
from Avizo by combining the distance maps with the thresholded voids.
raw 2D slicep
segmented voids
yarn distance map edge distance map
Outline Introduction Experimental Results Conclusion
X-ray Computed Tomography
Visualisation
The porosity distribution measurements in 3D are focussed on the
position of the voids relative to both the edges of the panel and the yarns.
The void-to-yarn distance and the void-to-edge distance can be obtained
from Avizo by combining the distance maps with the thresholded voids.
raw 2D slicep
segmented voids
yarn distance map
void-to-yarn distance map
edge distance map
Outline Introduction Experimental Results Conclusion
X-ray Computed Tomography
Visualisation
The porosity distribution measurements in 3D are focussed on the
position of the voids relative to both the edges of the panel and the yarns.
The distance of every voxel segmented as void to the closest yarn and the
closest edge can be measured over the entire 3D volume.
raw 2D slicep
segmented voids
yarn distance map
void-to-yarn distance map
edge distance map
void-to-edge distance map
Outline Introduction Experimental Results Conclusion
X-ray Computed Tomography
Visualisation
raw 2D slicep
segmented voids
yarn distance map
void-to-yarn distance map
edge distance map
void-to-edge distance map
Outline Introduction Experimental Results Conclusion
Void overview
Porosity Overview
Table 1: Summary of the void equivalent diameter1
.
Specimen Minimum Maximum Mean Standard deviation
label mm mm mm mm
L-1 0.027 0.398 0.078 0.055
L-2 0.027 0.404 0.075 0.050
L-3 0.027 0.290 0.073 0.049
H-1 0.027 0.406 0.078 0.055
H-2 0.027 0.458 0.074 0.051
H-3 0.027 0.419 0.083 0.059
1The equivalent diameter is the diameter the void would have if it was perfectly
spherical.
Outline Introduction Experimental Results Conclusion
Void overview
Porosity Overview
Table 1: Summary of the void equivalent diameter1
.
Specimen Minimum Maximum Mean Standard deviation
label mm mm mm mm
L-1 0.027 0.398 0.078 0.055
L-2 0.027 0.404 0.075 0.050
L-3 0.027 0.290 0.073 0.049
H-1 0.027 0.406 0.078 0.055
H-2 0.027 0.458 0.074 0.051
H-3 0.027 0.419 0.083 0.059
Minimum just below 0.03 mm and limited by resolution of XCT.
1The equivalent diameter is the diameter the void would have if it was perfectly
spherical.
Outline Introduction Experimental Results Conclusion
Void overview
Porosity Overview
Table 1: Summary of the void equivalent diameter1
.
Specimen Minimum Maximum Mean Standard deviation
label mm mm mm mm
L-1 0.027 0.398 0.078 0.055
L-2 0.027 0.404 0.075 0.050
L-3 0.027 0.290 0.073 0.049
H-1 0.027 0.406 0.078 0.055
H-2 0.027 0.458 0.074 0.051
H-3 0.027 0.419 0.083 0.059
Maximum equivalent diameter are around 0.40 mm.
1The equivalent diameter is the diameter the void would have if it was perfectly
spherical.
Outline Introduction Experimental Results Conclusion
Void overview
Porosity Overview
Table 1: Summary of the void equivalent diameter1
.
Specimen Minimum Maximum Mean Standard deviation
label mm mm mm mm
L-1 0.027 0.398 0.078 0.055
L-2 0.027 0.404 0.075 0.050
L-3 0.027 0.290 0.073 0.049
H-1 0.027 0.406 0.078 0.055
H-2 0.027 0.458 0.074 0.051
H-3 0.027 0.419 0.083 0.059
Mean void diameter ranges from 0.075 mm up to 0.084 mm.
1The equivalent diameter is the diameter the void would have if it was perfectly
spherical.
Outline Introduction Experimental Results Conclusion
Sample L (low viscosity resin)
Void size distribution
KS test on the three equivalent diameter distributions reveals that the
data are from the same continuous distribution.
Outline Introduction Experimental Results Conclusion
Sample L (low viscosity resin)
Void spatial distribution
Homogeneous distribution of voids through the panel thickness, the
evenly spaced maxima reflect the regular positions of the yarns.
Outline Introduction Experimental Results Conclusion
Sample L (low viscosity resin)
Void spatial distribution
Single sharp and intense peak at a distance close to 0.12 mm which
indicates that the voids are mainly located around the yarns.
Outline Introduction Experimental Results Conclusion
Sample H (high viscosity resin)
Void size distribution
KS test on the three equivalent diameter distributions reveals that the
data are from the same continuous distribution.
Outline Introduction Experimental Results Conclusion
Sample H (high viscosity resin)
Void spatial distribution
Peak intensities increase with increasing distance from the panel edge,
indicating a higher distribution of voids close to the centre of the panel.
Outline Introduction Experimental Results Conclusion
Sample H (high viscosity resin)
Void spatial distribution
Single sharp and intense peak at a distance close to 0.12 mm which
indicates that the voids are mainly located around the yarns.
Outline Introduction Experimental Results Conclusion
Sample comparison
Void size distribution
K-S test rejects the hypothesis that the two void distributions are from
the same distribution.
Outline Introduction Experimental Results Conclusion
Sample comparison
Void size distribution
K-S test rejects the hypothesis that the two void distributions are from
the same distribution.
Outline Introduction Experimental Results Conclusion
Sample comparison
Void spatial distribution – qualitative
Homogeneous void distribution for panel L and higher void distribution
close to the centre of panel H.
Outline Introduction Experimental Results Conclusion
Sample comparison
Void spatial distribution – qualitative
Similar sharp peak around 0.12 mm which indicates that the voids are
mainly located around the yarns for both specimens.
Outline Introduction Experimental Results Conclusion
Sample comparison
Void spatial distribution – quantitative
50 % of the voids lie within the middle 2.5 mm of panel L
50 % of the voids lie within the middle 0.5 mm of panel H
Outline Introduction Experimental Results Conclusion
Sample comparison
Void spatial distribution – quantitative
90 % of the voids are located within 0.25 mm from the yarns in panel L
90 % of the voids are located within 0.50 mm from the yarns in panel H
Outline Introduction Experimental Results Conclusion
Summary
Summary
Summary:
Composite panels have been manufactured by resin film infusion
The pore distribution in the panels has been fully characterised
Highlights:
No major difference between specimens with standard pore analysis
The void-to-yarn and void-to-edge distance maps showed major
differences between the panels:
Homogeneous void distribution for panel L and higher void
distribution close to the centre of panel H.
In both panels, the pores are mainly located around the yarns.
Both qualitative and quantitative analyses can be performed
Outline Introduction Experimental Results Conclusion
Discussion
Discussion
Questions ?
Fabien L´eonard
fabien.leonard@manchester.ac.uk

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3D Characterisation of Pore Distribution in Resin Film Infused Composites

  • 1. Outline Introduction Experimental Results Conclusion 3D Characterisation of Pore Distribution in Resin Film Infused Composites Fabien L´eonard1 , Jasmin Stein2 , Arthur Wilkinson2 , and Philip J. Withers1 1 Henry Moseley X-ray Imaging Facility, The University of Manchester 2 Northwest Composites Centre, The University of Manchester Industrial Computed Tomography September 20 th 2012 Wels, Austria
  • 2. Outline Introduction Experimental Results Conclusion Outline 1 Introduction Overview 2 Experimental Materials X-ray Computed Tomography 3 Results Void overview Sample L (low viscosity resin) Sample H (high viscosity resin) Sample comparison 4 Conclusion
  • 3. Outline Introduction Experimental Results Conclusion Overview Void assessment in composites The properties of a composite are detrimentally affected by voids introduced during the manufacturing process. The common method of determining the void volume fraction is acid digestion for carbon fibre reinforced composites and matrix burn off for glass fibre reinforced composites.
  • 4. Outline Introduction Experimental Results Conclusion Materials Specimen Manufacturing Epoxy resins: triglycidylaminophenol TGAP (Araldite MY0510, Huntsman) and tetraglycidyl-4,4’-diaminodiphenylmethane TGDDM (Araldite® MY721, Huntsman) Hardener: 4,4’-diaminophenyl sulfone, DDS (Aradur 976-1, Huntsman) Reinforcement: unidirectional carbon fibre fabric supplied by Sigmatex 12 k carbon tows were bound with a fine glass fibre yarn (spacing of approximately 6 mm to give a fabric of 445 g.m−2 )
  • 5. Outline Introduction Experimental Results Conclusion Materials Specimens Two composite panels were investigated in this study: Panel L was made from unmodified resin (low viscosity resin) Panel H was made from the same resin modified with polyethersulfone, PES (Virantage VW-10300 FP, Solvay) to improve fracture toughness (which results in a higher viscosity resin). Each panel (approximately 5 mm thick) was cut into five 25 mm wide strips, along the 0◦ direction.
  • 6. Outline Introduction Experimental Results Conclusion Materials Resin film infusion Composite laminates were manufactured by resin film infusion (RFI) which is suitable for high viscosity resins. Resin films were degassed at 130 ◦ C for 1 hour and then were immediately frozen. The laminates were cured for 2 hours at at 130 ◦ C, 165 ◦ C, and 200 ◦ C Vacuum was applied throughout the cycle for the infusion to take place.
  • 7. Outline Introduction Experimental Results Conclusion X-ray Computed Tomography Acquisition Scanning was performed at the Henry Moseley X-ray Imaging Facility on the Nikon Metrology 225/320 kV Custom Bay system: Voxel size: 17.3 µm Target: Cu Voltage: 75 kV Current: 130 µA Filter: none Exposure time: 2000 ms Number of projections: 3142 Acquisition time: 1h 45’
  • 8. Outline Introduction Experimental Results Conclusion X-ray Computed Tomography Visualisation The visualisation software employed was Visualisation Science Group proprietary software Avizo Fire version 7.0.1. The voids, matrix and yarns were segmented as follows:
  • 9. Outline Introduction Experimental Results Conclusion X-ray Computed Tomography Visualisation The visualisation software employed was Visualisation Science Group proprietary software Avizo Fire version 7.0.1. The voids, matrix and yarns were segmented as follows: Pores [0;60] voids only
  • 10. Outline Introduction Experimental Results Conclusion X-ray Computed Tomography Visualisation The visualisation software employed was Visualisation Science Group proprietary software Avizo Fire version 7.0.1. The voids, matrix and yarns were segmented as follows: Pores [0;60] Yarns [150;255] binder yarn and voids
  • 11. Outline Introduction Experimental Results Conclusion X-ray Computed Tomography Visualisation The visualisation software employed was Visualisation Science Group proprietary software Avizo Fire version 7.0.1. The voids, matrix and yarns were segmented as follows: Pores [0;60] Composite [60;150] Yarns [150;255] all labels y
  • 12. Outline Introduction Experimental Results Conclusion X-ray Computed Tomography Visualisation The porosity distribution measurements in 3D are focussed on the position of the voids relative to both the edges of the panel and the yarns. The void-to-yarn distance and the void-to-edge distance can be obtained from Avizo by combining the distance maps with the thresholded voids. raw 2D slicep
  • 13. Outline Introduction Experimental Results Conclusion X-ray Computed Tomography Visualisation The porosity distribution measurements in 3D are focussed on the position of the voids relative to both the edges of the panel and the yarns. The void-to-yarn distance and the void-to-edge distance can be obtained from Avizo by combining the distance maps with the thresholded voids. raw 2D slicep segmented voids
  • 14. Outline Introduction Experimental Results Conclusion X-ray Computed Tomography Visualisation The porosity distribution measurements in 3D are focussed on the position of the voids relative to both the edges of the panel and the yarns. The void-to-yarn distance and the void-to-edge distance can be obtained from Avizo by combining the distance maps with the thresholded voids. raw 2D slicep segmented voids yarn distance map edge distance map
  • 15. Outline Introduction Experimental Results Conclusion X-ray Computed Tomography Visualisation The porosity distribution measurements in 3D are focussed on the position of the voids relative to both the edges of the panel and the yarns. The void-to-yarn distance and the void-to-edge distance can be obtained from Avizo by combining the distance maps with the thresholded voids. raw 2D slicep segmented voids yarn distance map void-to-yarn distance map edge distance map
  • 16. Outline Introduction Experimental Results Conclusion X-ray Computed Tomography Visualisation The porosity distribution measurements in 3D are focussed on the position of the voids relative to both the edges of the panel and the yarns. The distance of every voxel segmented as void to the closest yarn and the closest edge can be measured over the entire 3D volume. raw 2D slicep segmented voids yarn distance map void-to-yarn distance map edge distance map void-to-edge distance map
  • 17. Outline Introduction Experimental Results Conclusion X-ray Computed Tomography Visualisation raw 2D slicep segmented voids yarn distance map void-to-yarn distance map edge distance map void-to-edge distance map
  • 18. Outline Introduction Experimental Results Conclusion Void overview Porosity Overview Table 1: Summary of the void equivalent diameter1 . Specimen Minimum Maximum Mean Standard deviation label mm mm mm mm L-1 0.027 0.398 0.078 0.055 L-2 0.027 0.404 0.075 0.050 L-3 0.027 0.290 0.073 0.049 H-1 0.027 0.406 0.078 0.055 H-2 0.027 0.458 0.074 0.051 H-3 0.027 0.419 0.083 0.059 1The equivalent diameter is the diameter the void would have if it was perfectly spherical.
  • 19. Outline Introduction Experimental Results Conclusion Void overview Porosity Overview Table 1: Summary of the void equivalent diameter1 . Specimen Minimum Maximum Mean Standard deviation label mm mm mm mm L-1 0.027 0.398 0.078 0.055 L-2 0.027 0.404 0.075 0.050 L-3 0.027 0.290 0.073 0.049 H-1 0.027 0.406 0.078 0.055 H-2 0.027 0.458 0.074 0.051 H-3 0.027 0.419 0.083 0.059 Minimum just below 0.03 mm and limited by resolution of XCT. 1The equivalent diameter is the diameter the void would have if it was perfectly spherical.
  • 20. Outline Introduction Experimental Results Conclusion Void overview Porosity Overview Table 1: Summary of the void equivalent diameter1 . Specimen Minimum Maximum Mean Standard deviation label mm mm mm mm L-1 0.027 0.398 0.078 0.055 L-2 0.027 0.404 0.075 0.050 L-3 0.027 0.290 0.073 0.049 H-1 0.027 0.406 0.078 0.055 H-2 0.027 0.458 0.074 0.051 H-3 0.027 0.419 0.083 0.059 Maximum equivalent diameter are around 0.40 mm. 1The equivalent diameter is the diameter the void would have if it was perfectly spherical.
  • 21. Outline Introduction Experimental Results Conclusion Void overview Porosity Overview Table 1: Summary of the void equivalent diameter1 . Specimen Minimum Maximum Mean Standard deviation label mm mm mm mm L-1 0.027 0.398 0.078 0.055 L-2 0.027 0.404 0.075 0.050 L-3 0.027 0.290 0.073 0.049 H-1 0.027 0.406 0.078 0.055 H-2 0.027 0.458 0.074 0.051 H-3 0.027 0.419 0.083 0.059 Mean void diameter ranges from 0.075 mm up to 0.084 mm. 1The equivalent diameter is the diameter the void would have if it was perfectly spherical.
  • 22. Outline Introduction Experimental Results Conclusion Sample L (low viscosity resin) Void size distribution KS test on the three equivalent diameter distributions reveals that the data are from the same continuous distribution.
  • 23. Outline Introduction Experimental Results Conclusion Sample L (low viscosity resin) Void spatial distribution Homogeneous distribution of voids through the panel thickness, the evenly spaced maxima reflect the regular positions of the yarns.
  • 24. Outline Introduction Experimental Results Conclusion Sample L (low viscosity resin) Void spatial distribution Single sharp and intense peak at a distance close to 0.12 mm which indicates that the voids are mainly located around the yarns.
  • 25. Outline Introduction Experimental Results Conclusion Sample H (high viscosity resin) Void size distribution KS test on the three equivalent diameter distributions reveals that the data are from the same continuous distribution.
  • 26. Outline Introduction Experimental Results Conclusion Sample H (high viscosity resin) Void spatial distribution Peak intensities increase with increasing distance from the panel edge, indicating a higher distribution of voids close to the centre of the panel.
  • 27. Outline Introduction Experimental Results Conclusion Sample H (high viscosity resin) Void spatial distribution Single sharp and intense peak at a distance close to 0.12 mm which indicates that the voids are mainly located around the yarns.
  • 28. Outline Introduction Experimental Results Conclusion Sample comparison Void size distribution K-S test rejects the hypothesis that the two void distributions are from the same distribution.
  • 29. Outline Introduction Experimental Results Conclusion Sample comparison Void size distribution K-S test rejects the hypothesis that the two void distributions are from the same distribution.
  • 30. Outline Introduction Experimental Results Conclusion Sample comparison Void spatial distribution – qualitative Homogeneous void distribution for panel L and higher void distribution close to the centre of panel H.
  • 31. Outline Introduction Experimental Results Conclusion Sample comparison Void spatial distribution – qualitative Similar sharp peak around 0.12 mm which indicates that the voids are mainly located around the yarns for both specimens.
  • 32. Outline Introduction Experimental Results Conclusion Sample comparison Void spatial distribution – quantitative 50 % of the voids lie within the middle 2.5 mm of panel L 50 % of the voids lie within the middle 0.5 mm of panel H
  • 33. Outline Introduction Experimental Results Conclusion Sample comparison Void spatial distribution – quantitative 90 % of the voids are located within 0.25 mm from the yarns in panel L 90 % of the voids are located within 0.50 mm from the yarns in panel H
  • 34. Outline Introduction Experimental Results Conclusion Summary Summary Summary: Composite panels have been manufactured by resin film infusion The pore distribution in the panels has been fully characterised Highlights: No major difference between specimens with standard pore analysis The void-to-yarn and void-to-edge distance maps showed major differences between the panels: Homogeneous void distribution for panel L and higher void distribution close to the centre of panel H. In both panels, the pores are mainly located around the yarns. Both qualitative and quantitative analyses can be performed
  • 35. Outline Introduction Experimental Results Conclusion Discussion Discussion Questions ? Fabien L´eonard fabien.leonard@manchester.ac.uk