In situ monitoring of SI-ATRP throughout multiple reinitiations under flow by means of a quartz crystal microbalance

Abstract

The polymerisation of 2-hydroxyethyl methacrylate (HEMA) by means of surface-initiated atom transfer radical polymerisation (SI-ATRP) has been studied in situ using a quartz crystal microbalance, with multiple reinitiations under continuous flow of the reaction mixture.

Synthesis of acrylamide-based block-copolymer brushes under flow: monitoring real-time growth and surface restructuring upon drying

“…The flow system is presented in Scheme 1. Although QCM-D has been successfully used by others, including ourselves, to study the growth kinetics of surface-initiated polymerization, 18,[20][21][22][23][24][25] in this study we have demonstrated that QCM-D can also be extremely useful in monitoring the real-time growth of block-copolymer brushes.…”

“…Therefore, the linear ΔF-t profiles corresponding to the polymerization of NIPAM, DMAM and HEAM clearly demonstrate a steady increase in the brush thickness as a result of the living nature of the SI-ATRP process-as we have previously reported for the homopolymers. 18,23 The sharp changes, however, while switching from one monomer to another, are caused by sudden changes in the viscosity of the medium. To rule out the possibility of the QCM-D profiles being affected by physisorption of the monomers, we also carried out a similar experiment with HEAM but in the absence of ATRP-catalyst and the result is presented in Fig.…”

Visualization of Atom Transfer Radical Polymerization by Aggregation‐Induced Emission Technology

“…Spencer et al. reported the using a quartz crystal microbalance for in‐situ investigation of surface‐initiated ATRP of 2‐hydroxyethyl methacrylate (HEMA) . Zhang et al.…”

“…Spencer et al reported the using a quartz crystal microbalance for in-situ investigation of surface-initiated ATRP of 2-hydroxyethyl methacrylate (HEMA). [6] Zhang et al used in-situ infrared spectroscopy (IR) to monitor the electron transfer ATRP polymerization process for copolymer of poly(hydroxyethyl methacrylate-co-tert-butyl methacrylate) [P(HEMA-co-tBMA)]. [7] Upon examination of the current status of method for monitoring the ATRP in situ and the major limitation of conventional means of detection, an apparent question arises: the paucity of methods for monitoring the ATRP in situ at the molecular level.…”

Tuning and in situ monitoring of surface-initiated, atom-transfer radical polymerization of acrylamide derivatives in water-based solvents

“…This technique was chosen because of its exceptional ability to monitor changes in the mass of the polymer films, as they grow in real time. [19][20][21] The polymerization was performed at room temperature from a monolayer of SI-ATRP initiator, immobilized onto the SiO 2 -coated QCM-D sensors. In brief, a baseline was first established by flowing 80 : 20 ethanol/water through the QCM-D cells; the medium was then switched to the complete reaction mixture (CRM; i.e.…”