In situ monitoring of mechanical properties during photopolymerization with particle tracking microrheology

Slopek, Ryan; McKinley, Haris K.; Henderson, Clifford L.; Breedveld, Victor

doi:10.1016/j.polymer.2006.01.095

Cited by 30 publications

(34 citation statements)

References 22 publications

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“…Ultraviolet (UV)‐visible (vis) photopolymerization is increasingly being used because of its advantages of fast polymerization and flexible reaction equipment. Traditional small‐molecule initiators are an important component of a polymerization reaction.…”

Section: Introductionmentioning

confidence: 99%

Synthesis of novel macrophotoinitiator for the photopolymerization of acrylate

Niu

et al. 2014

J of Applied Polymer Sci

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A new kind of macrophotoinitiator (MPI) was synthesized through the copolymerization of acrylic monomers and the polymerizable photoinitiator monomer 2959-AA. Monomer 2959-AA was obtained by an esterification reaction between acrylic acid (AA) and the water-soluble photoinitiator Irgacure 2959 [2-hydroxy-4-(2-hydroxyethoxy)-2-methylpropiophenone]. By adjusting the monomer proportions in the MPIs, two series of MPIs with different 2959-AA contents and different glass transition temperatures were obtained. The molecular structure of 2959-AA was characterized by Fourier-transform infrared spectroscopy, nuclear magnetic spectrometry, and mass spectrometry. Polymerization of 1, 6-hexanediol diacrylate was initiated using Irgacure 2959 and 2959-AA, and two series of MPIs to be polymerized were studied with a photo-DSC test. Results showed that 2959-AA had higher chemical reactivity than Irgacure 2959 because of the higher solubility of the former. It was evident from the experiments that 2959-AA content in the MPI progressively increased the polymerization rate and monomer conversion when the glass transition temperatures of MPIs were similar. At the same 2959-AA content, the polymerization rate slightly slowed down with increased glass transition temperature. However, the radical lifetime and polymerization time were prolonged.

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Section: Introductionmentioning

confidence: 99%

Synthesis of novel macrophotoinitiator for the photopolymerization of acrylate

Niu

et al. 2014

J of Applied Polymer Sci

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“…A more direct measurement of mechanical properties during photo‐induced free radical polymerization is preferable. Microrheological techniques can easily and directly detect changes in mechanical properties including the drastic increase in viscosity at the gelation point during photopolymerization, in contrast to traditional rheology techniques where bulk properties are measured and the sample is subjected to an externally imposed shear strain .…”

Section: Introductionmentioning

confidence: 99%

“…In this work, a kinetic and stochastic modeling of the photopolymerization process was performed that takes into account the molecular weight and crosslink density change. Such improvements in the theoretical models would greatly aid the process improvements where higher throughput, better spatial resolution, and improved surface finish are important, i.e., stereolithography . The objective of the models developed in this study is to model the critical degree of polymerization that results in gelation.…”

Section: Introductionmentioning

confidence: 99%

Simulation of models for multifunctional photopolymerization kinetics

Altun-Çiftçioğlu

Ersoy-Meriçboyu

Henderson

2013

Polymer Engineering & Sci

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In this study, two different models of photopolymerization of multifunctional monomers are developed. The first is a kinetic model and is based on first order nonlinear ordinary differential equations describing the rates of photoinitiator, monomer, and live and dead radicals of different chain lengths. In the second model, a stochastic Monte Carlo approach is used to predict the time evolution of the photopolymerization process. In this model the chain affects are incorporated both in the propagation and termination rate constants. The simulations of these models for the predictions of gelation times are compared with the experimental values measured in the absence of oxygen in the reaction volume by using passive microrheology technique. The nonlinear decrease of gelation time with increasing photoinitator concentration and number of acrylate fragments on each monomer is best captured with the second model. Furthermore, the second model is successfully verified with kinetic data generated from FTIR and DSC experiments. POLYM. ENG. SCI., 54:1737-1746

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“…Raman spectroscopy14 and nano‐indentation15 have been used to follow conversion and modulus, respectively, but not during photopolymerization. Particle tracking microrheology16 methods were used to characterize the gelation time of UV curing coatings as a function of depth during photopolymerization; however, this method did not provide real‐time photorheology information.…”

Section: Introductionmentioning

confidence: 99%

Depthwise Viscosity Gradients in UV‐Cured Epoxy Coatings

Song

McCormick

Francis

2012

Macro Materials & Eng

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A magnetic microrheometer is used to characterize the development of viscosity at different depths in UV‐cured epoxy coatings. Lateral magnetic particle velocities are tracked at different depths to quantify viscosity gradients. In general, viscosity build‐up is faster near the coating surface, tending to produce a “skin”. The effects of process conditions on the viscosity gradient development, on the rate of viscosity increase, and on surface defects are studied. More severe gradients develop in thicker coatings and in those with higher photoinitiator concentration. Under some conditions, the skin layer wrinkles, indicating the development of local compressive stress. Curing at higher temperature, however, increases cure rates while reducing the viscosity gradients and wrinkling defects.

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In situ monitoring of mechanical properties during photopolymerization with particle tracking microrheology

Cited by 30 publications

References 22 publications

Synthesis of novel macrophotoinitiator for the photopolymerization of acrylate

Synthesis of novel macrophotoinitiator for the photopolymerization of acrylate

Simulation of models for multifunctional photopolymerization kinetics

Depthwise Viscosity Gradients in UV‐Cured Epoxy Coatings

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