Fracture Behaviour and Damage
Characterisation in Composite Impact
Panels by Laboratory X-ray Computed
Tomography
Arthur Wilkinson1, Jasmin Stein1,2, Philip J. Withers2, and Fabien Léonard2
1Northwest Composite Centre, 2Henry Moseley X-ray Imaging Facility, School of Materials, The University of Manchester, UK

Thermosets 2013
September 18th – 20th , Berlin

NCCEF
Outline

Introduction

Experimental procedures

Results

Outline
•

Introduction
– Overview

•

Experimental procedures
– Materials
– Manufacturing
– Characterisation (SENB fracture, Mode-I ILFT, XCT)

•

Results
– Plane-Strain Fracture Toughness of Matrices
– XCT of As-prepared Panels
– Mode I Interlaminar Fracture Toughness
– Impact Behaviour
– XCT of Impact Damage

•

Conclusions

Conclusion
Outline

Experimental procedures

Introduction

Results

Conclusion

Materials

Base system
• Base System
– Formulated using Factorial Experiment Design (FED) based on;
• Tg
• Heat of reaction
• Viscosity
– Chemical structures;
(a) TGAP (Araldite® MY0510, Huntsman)

(b) TGDDM (Araldite® MY721, Huntsman)
O

O
CH2

O
CH2

CH

O

CH2

CH2

CH

O
CH

CH2

CH2
N

N

CH2

CH

CH2

CH2

CH

CH2

(c) DDS (Aradure® 976-1, Huntsman)
O

O
S

NH2

N

CH2

CH

CH2
O

O

O

CH2

CH2

CH

NH2
Outline

Experimental procedures

Introduction

Results

Conclusion

Materials

Toughening agents
• PES
(a) Reactive high molecular weight (47k) - Virantage® VW10200 RFP, Solvay
(b) Reactive low molecular weight (21k) - Virantage® VW10700 RFP , Solvay
(c) Non-reactive medium molecular weight (36k) - Virantage® VW10300 FP , Solvay
O

O
S

O
n

• Tri-block copolymer (dimethylacrylamide-modified) MAM
(a) Functional MAM -Nanostrength® M52N NP, Arkema

PMMA/DMA

PBuA

PMMA/DMA
Outline

Introduction

Experimental procedures

Results

Conclusion

Manufacturing

Cure cycle optimisation and RFI
220

2 hours

200
Temperature (ºC)

• Cure cycle
– Optimised cure cycle based
on the degree of cure of the
neat resin
– Degree of cure > 95 %

200°C

180

2 hours

165°C

160
140

2 hours

130°C

120
100
0

• Resin Film Infusion (RFI)

50

100

150

200
250
Time (min)

300

350

400

Vacuum Bag
Mesh
Perforated Release Film

20 µm Release Film

Peel Ply
Fabric Stack

Mode-I sample
Vacuum
Outlet

Resin Film

Tacky Tape

Tool
Breather Fabric

Stacks [90, 0, 90, 0] of UD carbon fibre fabric, of 445 gm-2(Sigmatex, UK).
12k carbon tows bound by a fine glass fibre weft yarn at ≈ 6 mm intervals
Outline

Introduction

Experimental procedures

Results

Conclusion

Characterisation

Techniques
• XCT
– Nikon Metrology 225/320 kV Custom Bay
(see www.mxif.manchester.ac.uk )

• Impact

• Acid digestion – void volume %
– ASTM D3171
– Matrix digestion using
sulfuric acid/ hydrogen peroxide
– Specimen size ≈1 g

– Instron Ceast 9350 Drop Tower
– 89 mm x 55 mm, energies 5,10,15, 20 J

• Plane-Strain Fracture Toughness -KIc
– ASTM D5045
– 44 mm x 10 mm x 5 mm
– at 10 mm/min crosshead speed

• Mode I Interlaminar Fracture
Toughness- GIc
– ASTM D5528
– 125 mm x 25 mm x 5 mm
– at 0.75 mm/min crosshead speed
Outline

Introduction

Experimental procedures

Results

Conclusion

Results

Composites
Table 1: Acid digestion results of manufactured laminates.
Laminates
with

Additive
wt. %

Fibre
Content
Vol. %

Void Content
Vol. %

Neat Resin

0

68.4 ± 0.4

0.67 ± 0.10

RHMW PES

10

67.4 ± 2.0

1.23 ± 0.26

NRMMW PES

10

68.9 ± 0.1

1.35± 0.32

RBCP

5

69.6 ± 0.5

2.09 ± 0.05

X-Ray CT

a) all labels

b) Glass weft
Yarns and voids

c) Voids only

Examples of segmentation: matrix (blue), yarn (yellow), and pores (red) (10 mm scale bar).
Outline

Introduction

Experimental procedures

Results

XCT statistical analysis of void positions

Probability density - void to yarn distance

Results

Conclusion
Outline

XCT

Introduction

Experimental procedures

Results

Conclusion
Outline

Introduction

Experimental procedures

Results

Conclusion

Comparative Rheology

All 5%
addition
Outline

Introduction

Experimental procedures

Results

Results

Plane-Strain Fracture Toughness of Bulk Matrices -KIc

Chosen as matrices

•Molecular weight ↑ - toughening effect ↑
•Reactivity - toughening effect ↓
•Tri-block copolymer has the greatest effect

Conclusion
Outline

Introduction

Results

Mode I Interlaminar Fracture

Experimental procedures

Results

Conclusion
Outline

Introduction

Experimental procedures

Results

Conclusion

Results

Mode I Interlaminar Fracture
RHMW

NRMMW

Mode-I initiation GIC values

Mean Mode-I propagation values

FBCP
Outline

Introduction

Experimental procedures

Results

Conclusion

Results

Impact

Cross-sectional orthoslice views (XZ, YZ) – unmodified resin system
Outline

Introduction

Experimental procedures

Results

Conclusion

Results

Impact

5J

15J

25J

Interfacial damage area progression with impact energy. The numbers indicate the
interlaminar regions below the impacted face – unmodified resin system
Outline

Introduction

Experimental procedures

Results

Conclusion

Results

Impact

15J

Unmodified resin

FBCP modified resin

15J
Outline

Introduction

Experimental procedures

Results

Conclusion

Results

Impact

FBCP
15J

3-D view of impact damage; each interfacial damage is given a different colour
Outline

Introduction

Experimental procedures

Results

Conclusion

Results

Impact

Damage volume vs. distance from impact face - unmodified resin 15J
Outline

Introduction

Experimental procedures

Results

Conclusion

Results

Impact

Damage volume vs. distance from impact face - different matrices 15J
Outline

Introduction

Experimental procedures

Results

Conclusion

Conclusions

• XCT can provide extension information on voids in as-prepared
composites and on damage in impacted composites.
• In the bulk matrix systems, FBCP imparted superior toughness
than PES.
•

In interlaminar fracture and impact testing differences due to matrix
fracture toughness become less clear.
Outline

Introduction

Experimental procedures

Results

Conclusion

Acknowledgements
• EPSRC – funding

• NWCC / NCCEF – facilities

• Alan Nesbitt – technical support

NCCEF – see www.nccef.co.uk

• Huntsman, Solvay, Sigmatex, Arkema – supply of materials

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Fracture behaviour and damage characterisation in composite impact panels by laboratory X-ray computed tomography