Monitoring real‐time curing of epoxies in situ using single‐sided NMR

Kelley, Mackenzie; Abdol, Nastaran; Soroushian, Parviz; Keating, Kristina; Balachandra, Anagi M.; Meldrum, Tyler

doi:10.1002/pol.20190117

Title: Monitoring real‐time curing of epoxies in situ using single‐sided NMR

Abstract

Abstract Adhesively bonded joints using epoxy are widely used in aircraft and aerospace structures. Quality control and defect detection during epoxy curing in such applications is critical. We used single‐sided nuclear magnetic resonance (NMR) to nondestructively probe and spatially resolve the change in the characteristic NMR relaxation time ( T ₂ ) of epoxies during curing on a substrate. Time‐dependent T ₂ values were fit to a Weibull function to model temporal changes in the NMR measurables. Our results demonstrate that the reduction in molecular mobility of various epoxy/curing agent mixtures occurs more rapidly at the interface than in the bulk. Further use of single‐sided NMR to acquire spatially resolved T ₂ data will provide a route for elucidatory epoxy curing studies. © 2020 Wiley Periodicals, Inc. J. Polym. Sci. 2020 , 58 , 616–623

Authors:

^[1]; Abdol, Nastaran ^[2]; Soroushian, Parviz ^[2];

^[3];

^[2];

^[1]

Department of Chemistry William &, Mary Williamsburg Virginia
Metna, Co. Lansing Michigan
Department of Earth and Environmental Sciences Rutgers University Newark New Jersey

Publication Date:: Tue Jan 21 00:00:00 EST 2020

Sponsoring Org.:: USDOE

OSTI Identifier:: 1592799

Resource Type:: Publisher's Accepted Manuscript

Journal Name:: Journal of Polymer Science

Additional Journal Information:: Journal Name: Journal of Polymer Science Journal Volume: 58 Journal Issue: 4; Journal ID: ISSN 2642-4150

Publisher:: Wiley Blackwell (John Wiley & Sons)

Country of Publication:: United States

Language:: English

Citation Formats


                    Kelley, Mackenzie, Abdol, Nastaran, Soroushian, Parviz, Keating, Kristina, Balachandra, Anagi M., and Meldrum, Tyler. Monitoring real‐time curing of epoxies in situ using single‐sided NMR.  United States: N. p., 2020. 
Web.  doi:10.1002/pol.20190117.

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                    Kelley, Mackenzie, Abdol, Nastaran, Soroushian, Parviz, Keating, Kristina, Balachandra, Anagi M., & Meldrum, Tyler. Monitoring real‐time curing of epoxies in situ using single‐sided NMR.  United States.  https://doi.org/10.1002/pol.20190117

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                    Kelley, Mackenzie, Abdol, Nastaran, Soroushian, Parviz, Keating, Kristina, Balachandra, Anagi M., and Meldrum, Tyler. Tue .  
"Monitoring real‐time curing of epoxies in situ using single‐sided NMR".  United States.  https://doi.org/10.1002/pol.20190117.

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@article{osti_1592799,

  title        = {Monitoring real‐time curing of epoxies in situ using single‐sided NMR},

  author       = {Kelley, Mackenzie and Abdol, Nastaran and Soroushian, Parviz and Keating, Kristina and Balachandra, Anagi M. and Meldrum, Tyler},

  abstractNote = {Abstract Adhesively bonded joints using epoxy are widely used in aircraft and aerospace structures. Quality control and defect detection during epoxy curing in such applications is critical. We used single‐sided nuclear magnetic resonance (NMR) to nondestructively probe and spatially resolve the change in the characteristic NMR relaxation time ( T 2 ) of epoxies during curing on a substrate. Time‐dependent T 2 values were fit to a Weibull function to model temporal changes in the NMR measurables. Our results demonstrate that the reduction in molecular mobility of various epoxy/curing agent mixtures occurs more rapidly at the interface than in the bulk. Further use of single‐sided NMR to acquire spatially resolved T 2 data will provide a route for elucidatory epoxy curing studies. © 2020 Wiley Periodicals, Inc. J. Polym. Sci. 2020 , 58 , 616–623},

  doi          = {10.1002/pol.20190117},

  journal      = {Journal of Polymer Science},

  number       = 4,

  volume       = 58,

  place        = {United States},

  year         = {Tue Jan 21 00:00:00 EST 2020},

  month        = {Tue Jan 21 00:00:00 EST 2020}

}

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Works referenced in this record:

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Title: Monitoring real‐time curing of epoxies in situ using single‐sided NMR

Abstract

Citation Formats

Environmental and chemical degradation of carbon/epoxy lap joints for aerospace applications, and effects on their mechanical performance journal, May 2010

Development of epoxy mixtures for application in aeronautics and aerospace journal, January 2014

Relaxation times and in situ kinetic analysis during network evolution of epoxy via a nickel catalyst of imidazole journal, March 2011

Modified Spin‐Echo Method for Measuring Nuclear Relaxation Times journal, August 1958

Profiles with microscopic resolution by single-sided NMR journal, September 2005

Observation of Interfacial Damage in a Silk-Epoxy Composite, Using a Simple Mechanoresponsive Fluorescent Probe journal, March 2017

Determination of crosslink density in thermoset polymers by use of solid-state proton NMR techniques journal, September 1988

Reduced interfacial adhesion in glass fibre-epoxy composites due to water absorption via molecular dynamics simulations journal, March 2019

Autoacceleration and inhibition: Free volume. Epoxy-amine kinetics journal, April 1998

Glass transition temperature as a function of conversion in thermosetting polymers journal, April 1991

Solving Fredholm integrals of the first kind with tensor product structure in 2 and 2.5 dimensions journal, May 2002

Mechanistic kinetic model of an epoxy resin cured with a mixture of amines of different functionalities journal, September 2005

NMR of Multipolar Spin States Excitated in Strongly Inhomogeneous Magnetic Fields journal, January 2002

Combined experimental/numerical investigation of directional moisture diffusion in glass/epoxy composites journal, October 2017

Double-Quantum-Filtered NMR Signals in Inhomogeneous Magnetic Fields journal, April 2001

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The nature of the structural gradient in epoxy curing at a glass fiber/epoxy matrix interface using FTIR imaging journal, November 2003

Real-time cure monitoring of an epoxy/polyamidoamine system with unilateral magnetic resonance journal, May 2011

Pulsed NMR Study of the Curing Process of Epoxy Resin journal, January 2008

Ultrasound monitoring of the cure kinetics of an epoxy resin: Identification, frequency and temperature dependence journal, December 2016

Simultaneous measurements of T1 and T2 during fast polymerization reaction using continuous wave-free precession NMR method: Simultaneous measurements of T1 and T2 during fast polymerization reaction using continuous wave-free precession NMR method journal, June 2012

Cure Kinetics Study of Two Epoxy Systems with Fourier Tranform Infrared Spectroscopy (FTIR) and Differential Scanning Calorimetry (DSC) journal, August 2012

Study of the moisture/stress effects on glass fibre/epoxy composite and the impact of the interphase area journal, February 2014

ICTAC Kinetics Committee recommendations for performing kinetic computations on thermal analysis data journal, June 2011

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Translational Dynamics and Magnetic Resonance: Principles of Pulsed Gradient Spin Echo NMR book, September 2011

Experimental study of silicone-epoxy dual adhesive joints for high temperature aerospace applications journal, May 2011

Multiple-Pulse Nuclear Magnetic Resonance Experiments on Some Crystalline Polymers journal, July 1972

A review of extending performance of epoxy resins using carbon nanomaterials journal, March 2018

Cure behaviors and mechanical properties of carbon fiber-reinforced nylon6/epoxy blended matrix composites journal, March 2017

Mobile single-sided NMR journal, May 2008

Pulsed NMR studies of crosslinking and entanglements in high molecular weight linear polydimethylsiloxanes journal, January 1977

Reaction Kinetics of Epoxy/Amine Model Systems. The Effect of Electrophilicity of Amine Molecule journal, December 1994

Kinetic methods to study isothermal and nonisothermal epoxy-anhydride cure journal, October 1999

Fluorescence Monitoring of Curing Process and Water Accessibility at Glass Fiber/Epoxy Interphase on Composite Materials journal, May 2001

Analysis of solid technical polymers by compact NMR journal, October 2016

The effect of network architecture on the thermal and mechanical behavior of epoxy resins journal, June 1998

Interphase formation in model composites studied by micro-thermal analysis journal, August 2002

Effects of Diffusion on Free Precession in Nuclear Magnetic Resonance Experiments journal, May 1954

Environmental and chemical degradation of carbon/epoxy lap joints for aerospace applications, and effects on their mechanical performance
journal, May 2010

Development of epoxy mixtures for application in aeronautics and aerospace
journal, January 2014

Relaxation times and in situ kinetic analysis during network evolution of epoxy via a nickel catalyst of imidazole
journal, March 2011

Modified Spin‐Echo Method for Measuring Nuclear Relaxation Times
journal, August 1958

Profiles with microscopic resolution by single-sided NMR
journal, September 2005

Observation of Interfacial Damage in a Silk-Epoxy Composite, Using a Simple Mechanoresponsive Fluorescent Probe
journal, March 2017

Determination of crosslink density in thermoset polymers by use of solid-state proton NMR techniques
journal, September 1988

Reduced interfacial adhesion in glass fibre-epoxy composites due to water absorption via molecular dynamics simulations
journal, March 2019

Autoacceleration and inhibition: Free volume. Epoxy-amine kinetics
journal, April 1998

Glass transition temperature as a function of conversion in thermosetting polymers
journal, April 1991

Solving Fredholm integrals of the first kind with tensor product structure in 2 and 2.5 dimensions
journal, May 2002

Mechanistic kinetic model of an epoxy resin cured with a mixture of amines of different functionalities
journal, September 2005

NMR of Multipolar Spin States Excitated in Strongly Inhomogeneous Magnetic Fields
journal, January 2002

Combined experimental/numerical investigation of directional moisture diffusion in glass/epoxy composites
journal, October 2017

Double-Quantum-Filtered NMR Signals in Inhomogeneous Magnetic Fields
journal, April 2001

Direct Correlation between Adsorption Energetics and Nuclear Spin Relaxation in a Liquid-saturated Catalyst Material
journal, July 2018

The nature of the structural gradient in epoxy curing at a glass fiber/epoxy matrix interface using FTIR imaging
journal, November 2003

Real-time cure monitoring of an epoxy/polyamidoamine system with unilateral magnetic resonance
journal, May 2011

Pulsed NMR Study of the Curing Process of Epoxy Resin
journal, January 2008

Ultrasound monitoring of the cure kinetics of an epoxy resin: Identification, frequency and temperature dependence
journal, December 2016

Simultaneous measurements of T1 and T2 during fast polymerization reaction using continuous wave-free precession NMR method: Simultaneous measurements of T1 and T2 during fast polymerization reaction using continuous wave-free precession NMR method
journal, June 2012

Cure Kinetics Study of Two Epoxy Systems with Fourier Tranform Infrared Spectroscopy (FTIR) and Differential Scanning Calorimetry (DSC)
journal, August 2012

Study of the moisture/stress effects on glass fibre/epoxy composite and the impact of the interphase area
journal, February 2014

ICTAC Kinetics Committee recommendations for performing kinetic computations on thermal analysis data
journal, June 2011

Effect of crosslinks on the glass transition temperature of end-linked elastomers
journal, July 1992

Translational Dynamics and Magnetic Resonance: Principles of Pulsed Gradient Spin Echo NMR
book, September 2011

Experimental study of silicone-epoxy dual adhesive joints for high temperature aerospace applications
journal, May 2011

Multiple-Pulse Nuclear Magnetic Resonance Experiments on Some Crystalline Polymers
journal, July 1972

A review of extending performance of epoxy resins using carbon nanomaterials
journal, March 2018

Cure behaviors and mechanical properties of carbon fiber-reinforced nylon6/epoxy blended matrix composites
journal, March 2017

Mobile single-sided NMR
journal, May 2008

Pulsed NMR studies of crosslinking and entanglements in high molecular weight linear polydimethylsiloxanes
journal, January 1977

Reaction Kinetics of Epoxy/Amine Model Systems. The Effect of Electrophilicity of Amine Molecule
journal, December 1994

Kinetic methods to study isothermal and nonisothermal epoxy-anhydride cure
journal, October 1999

Fluorescence Monitoring of Curing Process and Water Accessibility at Glass Fiber/Epoxy Interphase on Composite Materials
journal, May 2001

Analysis of solid technical polymers by compact NMR
journal, October 2016

The effect of network architecture on the thermal and mechanical behavior of epoxy resins
journal, June 1998

Interphase formation in model composites studied by micro-thermal analysis
journal, August 2002

Effects of Diffusion on Free Precession in Nuclear Magnetic Resonance Experiments
journal, May 1954