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Real-time polymerization monitoring in a dual-cured resin cement by magnetic resonance

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Abstract

The polymerization process of the dual-cured resin cement AllCem (FGM, Joinvile, Brazil) was investigated by unilateral nuclear magnetic resonance (NMR-MOUSE) and electron paramagnetic resonance (EPR). The NMR experiment allows measurements of the mobile monomers as function of time and depth, while real-time X-band EPR monitoring gives information about the concentration of free radicals. The monomer concentration instantly decays for photo-cured samples, but it remains constant about ~4 min for self-cured samples before starting to decrease. For the self-cured sample, the concentration of free radicals suddenly decreases to zero and then reappears with a strongly increasing rate. Models for the polymerization kinetics of each initiation protocol are proposed, giving insight into the polymerization process of the dual-cured resin cement.

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Abbreviations

I :

Initiator

A :

Amine

M :

Monomer unit

R :

Radical

\({\text{RM}}_{n}^{ *}\) :

Active macroradical

A * :

Amine radical

I * :

Initiator radical

\({\text{RM}}_{{n,{\text{b}}}}^{ *}\) :

Trapped macroradical with n monomer units

Z :

Inhibitor

D n+m :

“Dead” polymer containing n + m monomer units

k d :

Initiator decomposition rate constant

k p :

Propagation rate constant

k t :

Termination rate constant

k b :

Radical trapping rate constant

k z :

Inhibition rate constant

f 1 and f 2 :

Efficiency factors

CQ:

Camphorquinone

I 0 :

The intensity of light absorbed in the surface

φ :

Extinction coefficient

α :

Initiation efficiency

d :

The length of the light path in the sample

R PR :

Rate of production of primary radicals

β :

Fraction of exciplex forming free radicals

R P :

Rate of propagation

R t :

Rate of termination

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Acknowledgements

The authors thank the FGM Produtos Odontológicos Ltda (Joinvile, SC, Brazil) for providing dental materials. The author AMN thanks Brazilian National Council for Scientific and Technological Development (CNPQ) for financial support (Grant No. 290010/2009-8).

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Authors and Affiliations

  1. Departmento de Física, Universidade Estadual de Londrina, Rodovia PR-445 Km 380, Londrina, 86057-970, Brazil

    Bruno Luiz Santana Vicentin & Eduardo Di Mauro

  2. Institute of Technical and Macromolecular Chemistry, RWTH Aachen University, Worringerweg 1-2, 52074, Aachen, Germany

    Antonio Marchi Netto & Bernhard Blümich

  3. Departmento de Química, Universidade Estadual de Londrina, Rodovia PR-445 Km 380, Londrina, 86057-970, Brazil

    Luiz Henrique Dall’Antonia

Authors
  1. Bruno Luiz Santana Vicentin
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  2. Antonio Marchi Netto
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  3. Luiz Henrique Dall’Antonia
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  4. Eduardo Di Mauro
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  5. Bernhard Blümich
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Correspondence to Bruno Luiz Santana Vicentin.

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Vicentin, B.L.S., Netto, A.M., Dall’Antonia, L.H. et al. Real-time polymerization monitoring in a dual-cured resin cement by magnetic resonance. Polym. Bull. 74, 5163–5179 (2017). https://doi.org/10.1007/s00289-017-2007-1

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  • DOI: https://doi.org/10.1007/s00289-017-2007-1

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