2 200 university avenue west, waterloo, on, canada n2l 3g1 ... · aaron law1, leonardo simon2,...

1
Acknowledgements This work was supported by General Motors Corp. and the ORDCF Center for Automotive Materials and Manufacturing (CAMM). Special thanks to J. Tang, P. Dasappa, J. Mui, P. Kruger, A. Shin and D. Jürgen-Lohmann for laboratory support. Conclusions Crystallinity increased during aging at elevated temperature through increased chain mobility. Plastic deformations are concentrated within the matrix phase. The deformations are non-recoverable after the stresses are released. Future Work: In-situ monitoring of progressive failure mechanisms for a range of thermo-mechanical loading conditions. Contact: Dr. Pearl Lee-Sullivan Dr. Leonardo Simon Professor, University of Waterloo Assistant Professor, University of Waterloo Phone: (519) 888-4522 Phone: (519) 888-4567 ext. 33301 E-mail: [email protected] E-mail: [email protected] Objectives This work is part of a larger experimental program aimed at characterizing the creep response of GMT materials. As the polypropylene matrix is inherently viscoelastic, it is necessary to determine if the matrix material will be significantly affected by creep loading at elevated temperature. Scope 1. To characterize the effects of thermal aging (long-term exposure) on the iPP matrix phase of a GMT: - crystallinity changes, secondary crystallization - degradation, formation of oxidation products 2. To measure microscopic level creep deformation of composite due to combined stresses and temperatures: - in-situ imaging of creep deformation - identify the deformation regions (matrix areas or interface/interphase) Introduction Glass-Mat Thermoplastic (GMT) composite materials are increasingly being used in the automotive industry due to its high strength-to-weight ratio and ease of processing. Application – 3D semi-structural parts such as seat frames, wheel wells and under body panels. Materials – Commercial grade isotactic polypropylene (iPP) matrix reinforced with approximately 40% wt. short- or long/continuous- random glass-fibre mats* Methods To characterize the effects of thermal aging on extracted iPP matrix: Aging at 90 and 140 o C with different morphologies Wide-angle X-ray diffraction (WXRD) and Fourier Transform infrared spectroscopy (FTIR) were used to detect crystallinity and chemical changes To measure creep deformations: Polished specimens, cut from as-received molded composite plaques according to ASTM-1708-02a Miniature tensile tester, optical microscope and scanning electron microscope (SEM) were used for observations Results Crystallinity determined quantitatively from WXRD results showed increase in crystallinity after aging at both temperatures due to reduced area of amorphous-halo. FTIR data also showed increase in crystallinity at both temperature levels but oxidation products detected for sampled aged at 140 °C. Avrami plots showed the kinetics of secondary crystallization for samples with different morphologies. Crystallization was accelerated when aging at 140 °C due to oxidation chain scission – the shorter chains facilitated secondary crystallization. Creep deformation observed under optical microscope. Deformation mechanism (plastic and/or elastic): Propagated through the matrix/fibre interface Matrix shear deformation; indentation shows that the shear deformation in matrix phase is transverse to the general fibre orientation; interfacial cracks are minimal Characterization of Characterization of Microscale Microscale Deformations due to Creep Deformations due to Creep in Glass in Glass - - Mat Thermoplastic (GMT) Composites at Elevated Temperature Mat Thermoplastic (GMT) Composites at Elevated Temperature Aaron Law 1 , Leonardo Simon 2 , Pearl Lee-Sullivan 1 1 Department of Mechanical and Mechatronic Engineering and 2 Department of Chemical Engineering, University of Waterloo 200 University Avenue West, Waterloo, ON, Canada N2L 3G1 Avrami plots with Avrami exponents (reported in figure) aging for 12 days in 90 °C (left) and 140 °C (below). FTIR spectrum of development of carbonyl groups (1900- 1600 cm -1 ) aged for 12 days in a) 90 °C and b) 140 °C. Miniature tensile tester with environmental chamber was placed under an optical microscope (50X magnification) for in-situ measurement of creep deformation at different stress and elevated temperature levels. FTIR with thin film sample aged in heating stage allowed in-situ scanning of crystallinity changes and formation of oxidation products over the course of elevated temperature aging. * Source: Ericson M. and Berglund L., Composites Science and Technology, Vol. 43, 1992 Machined (left) and polished (right) microtensile specimens for creep testing under optical microscope for in-situ imaging under creep laoding. 1600 1650 1700 1750 1800 1850 1900 Wavenumber (cm -1 ) Absorbance (Arbitrary Units) a) b) Day 1 Day 2 Day 3 Day 4 Day 5 Day 6 to 12 Day 0 WXRD data of controlled cooling sample aged for 12 days in 90 and 140 o C. 0.02 0.022 0.024 0.026 0.028 0.03 0.032 0.034 0.036 0.038 0.04 -0.5 0 0.5 1 1.5 2 2.5 3 log(t/hr) log(-Ln(1-Xv)) Controlled Cooling n=3.7x10 -3 Ice Quenched n=3.0x10 -3 -0.12 -0.1 -0.08 -0.06 -0.04 -0.02 0 0.02 0.04 -0.5 0 0.5 1 1.5 2 2.5 3 log(t/hr) log(-Ln(1-Xv)) Ice Quenched n=5.4x10 -3 Ice Quenched n=68.5x10 -3 Ice Quenched n=7.6x10 -3 Controlled Cooling n=4.8x10 -3 Controlled Cooling n=137.3x10 -3 Controlled Cooling n= -0.7x10 -3 Indented and polished GMT PP/glass specimen under creep at 40 MPa and 80 °C for 0 hrs (left), 1 hr (centre) and 5 hrs (right) at 50X magnification, loaded in-plane. Polished GMT PP/glass specimen under creep loading at 20 MPa and 80 °C for 0 hrs (left) and 24 hrs (right) at 50X magnification. Sample is loaded in-plane. IPR 2007

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Page 1: 2 200 University Avenue West, Waterloo, ON, Canada N2L 3G1 ... · Aaron Law1, Leonardo Simon2, Pearl Lee-Sullivan1 1Department of Mechanical and Mechatronic Engineering and 2Department

AcknowledgementsThis work was supported by General Motors Corp. and the ORDCF Center for Automotive Materials and Manufacturing (CAMM). Special thanks to J. Tang, P. Dasappa, J. Mui, P. Kruger, A. Shin and D. Jürgen-Lohmann for laboratory support.

ConclusionsCrystallinity increased during aging at elevated temperature through increased chain mobility.

Plastic deformations are concentrated within the matrix phase. The deformations are non-recoverable after the stresses are released.

Future Work: In-situ monitoring of progressive failure mechanisms for a range of thermo-mechanical loading conditions.

Contact:Dr. Pearl Lee-Sullivan Dr. Leonardo SimonProfessor, University of Waterloo Assistant Professor, University of Waterloo

Phone: (519) 888-4522 Phone: (519) 888-4567 ext. 33301E-mail: [email protected] E-mail: [email protected]

ObjectivesThis work is part of a larger experimental program aimed at characterizing the creep response of GMT materials. As the polypropylene matrix is inherently viscoelastic, it is necessary to determine if the matrix material will be significantly affected by creep loading at elevated temperature.

Scope1. To characterize the effects of thermal aging (long-term

exposure) on the iPP matrix phase of a GMT:- crystallinity changes, secondary crystallization- degradation, formation of oxidation products

2. To measure microscopic level creep deformation of composite due to combined stresses and temperatures:- in-situ imaging of creep deformation- identify the deformation regions (matrix areas or interface/interphase)

IntroductionGlass-Mat Thermoplastic (GMT) composite materials are increasingly being used in the automotive industry due to its high strength-to-weight ratio and ease of processing.

Application – 3D semi-structural parts such as seat frames, wheel wells and under body panels.

Materials – Commercial grade isotactic polypropylene (iPP) matrix reinforced with approximately 40% wt. short-or long/continuous- random glass-fibre mats*

MethodsTo characterize the effects of thermal aging on extracted iPP matrix:

Aging at 90 and 140 oC with different morphologies

Wide-angle X-ray diffraction (WXRD) and Fourier Transform infrared spectroscopy (FTIR) were used to detect crystallinity and chemical changes

To measure creep deformations:

Polished specimens, cut from as-received moldedcomposite plaques according to ASTM-1708-02a

Miniature tensile tester, optical microscope and scanning electron microscope (SEM) were used for observations

ResultsCrystallinity determined quantitatively from WXRD results showed increase in crystallinity after aging at both temperatures due to reduced area of amorphous-halo.

FTIR data also showed increase in crystallinity at both temperature levels but oxidation products detected for sampled aged at 140 °C.

Avrami plots showed the kinetics of secondary crystallization for samples with different morphologies. Crystallization was accelerated when aging at 140 °C due to oxidation chain scission – the shorter chains facilitated secondary crystallization.

Creep deformation observed under optical microscope. Deformation mechanism (plastic and/or elastic):

Propagated through the matrix/fibre interface

Matrix shear deformation; indentation shows that the shear deformation in matrix phase is transverse to the general fibre orientation; interfacial cracks are minimal

Characterization of Characterization of MicroscaleMicroscale Deformations due to Creep Deformations due to Creep in Glassin Glass--Mat Thermoplastic (GMT) Composites at Elevated Temperature Mat Thermoplastic (GMT) Composites at Elevated Temperature

Aaron Law1, Leonardo Simon2, Pearl Lee-Sullivan1

1Department of Mechanical and Mechatronic Engineering and 2Department of Chemical Engineering, University of Waterloo 200 University Avenue West, Waterloo, ON, Canada N2L 3G1

Avrami plots with Avramiexponents (reported in figure) aging for 12 days in 90 °C (left) and 140 °C (below).

FTIR spectrum of development of carbonyl groups (1900-

1600 cm-1) aged for 12 days in a) 90 °C and b) 140 °C.

Miniature tensile tester with environmental chamber was placed under an optical microscope (50X magnification) for in-situ measurement of creep deformation at different stress and elevated temperature levels.

FTIR with thin film sample aged in heating stage allowed in-situ scanning of crystallinity changes and formation of oxidation products over the course of elevated temperature aging.

* Source: Ericson M. and Berglund L., Composites Science and Technology, Vol. 43, 1992

Machined (left) and polished (right) microtensile specimens for creep testing under optical microscope for in-situ imaging

under creep laoding.

1600165017001750180018501900Wavenumber (cm-1)

Abs

orba

nce

(Arb

itrar

y U

nits

)

a)

b)

Day 1

Day 2

Day 3

Day 4Day 5

Day 6 to 12

Day 0

WXRD data of controlled cooling sample aged for 12 days in 90 and 140oC.

0.02

0.022

0.024

0.026

0.028

0.03

0.032

0.034

0.036

0.038

0.04

-0.5 0 0.5 1 1.5 2 2.5 3

log(t/hr)

log(

-Ln(

1-Xv

))

Controlled Coolingn=3.7x10-3

Ice Quenched n=3.0x10-3

-0.12

-0.1

-0.08

-0.06

-0.04

-0.02

0

0.02

0.04

-0.5 0 0.5 1 1.5 2 2.5 3log(t/hr)

log(

-Ln(

1-Xv

))

Ice Quenchedn=5.4x10-3

Ice Quenchedn=68.5x10-3

Ice Quenchedn=7.6x10-3

Controlled Coolingn=4.8x10-3

Controlled Coolingn=137.3x10-3

Controlled Coolingn= -0.7x10-3

Indented and polished GMT PP/glass specimen under creep at 40 MPa and 80 °C for 0 hrs (left), 1 hr (centre) and 5 hrs (right) at 50X magnification, loaded in-plane.

Polished GMT PP/glass specimen under creep loading at 20 MPa and 80 °C for 0 hrs (left) and 24 hrs (right) at 50X magnification. Sample is loaded in-plane.

IPR 20

07