Probing the Glass Transition Temperature of Poly（vinyl butyral） Using Fluorescence Lifetime

doi:10.19894/j.issn.1000-0518.250188

Chinese Journal of Applied Chemistry ›› 2025, Vol. 42 ›› Issue (10): 1323-1334.DOI: 10.19894/j.issn.1000-0518.250188

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Probing the Glass Transition Temperature of Poly（vinyl butyral） Using Fluorescence Lifetime

Yu LI¹^,², Jiao MU³, Du-Jin WANG¹^,², Guo-Ming LIU¹^,²()

^1.CAS Key Laboratory of Engineering Plastics，Institute of Chemistry，Chinese Academy of Sciences，Beijing 100190，China
^2.University of Chinese Academy of Sciences，Beijing 100049，China
^3.Analysis and Test Center，Institute of Chemistry，Chinese Academy of Sciences，Beijing 100190，China

Received:2025-05-08 Accepted:2025-08-05 Published:2025-10-01 Online:2025-10-29
Contact: Guo-Ming LIU
About author:gmliu@iccas.ac.cn
Supported by:
the National Natural Science Foundation of China(21922308)

Abstract

Abstract:

Poly（vinyl butyral）（PVB） is widely used in laminated glass due to its excellent optical transmittance and adhesion. Measuring the glass transition temperature （T_g） of amorphous polymers is critically important. In this study， rhodamine B was grafted onto PVB chains as a fluorescent probe. By combining laser confocal microscopy with fluorescence lifetime imaging （FLIM）， the T_g of PVB was characterized using the intersection point of fluorescence lifetime versus temperature curves. Comparison with differential scanning calorimetry （DSC） results showed that the T_g of the blend with mass fraction 2% PVB-Rhb measured by fluorescence lifetime was in perfect agreement with that obtained via DSC， thus verifying the accuracy and sensitivity of the fluorescence method for T_g determination. Concurrently， this method is extended to thin film systems. The effects of fluorescent probe concentration and sample thickness on T_g were systematically investigated， revealing a quantitative correlation between the film thickness and T_g. T_g increased with reduced PVB film thickness. These results demonstrate FLIM as a robust tool for polymer T_g measurement， with advantages for characterization of substrate-supported polymer films and polymers in confined environments.

Key words: Laser confocal microscopy, Fluorescence lifetime imaging, Ultra-thin films, Glass transition temperature

CLC Number:

O631.2

Yu LI, Jiao MU, Du-Jin WANG, Guo-Ming LIU. Probing the Glass Transition Temperature of Poly（vinyl butyral） Using Fluorescence Lifetime[J]. Chinese Journal of Applied Chemistry, 2025, 42(10): 1323-1334.

Figures/Tables 11

Fig.1 Synthesis route for PVB-Rhb

Fig.2 The molecular formula of PVB

Fig.3 1H NMR spectrum of PVB in DMSO-d6

Fig.4 1H NMR spectrum of PVB-Rhb in DMSO-d6

Fig.5 1H NMR spectrum of Rhb （a）， PVB （b） and PVB-Rhb （c） in DMSO-d6

Fig.6 Ultraviolet absorption （UV） and fluorescence emission spectra （PL） of PVB-Rhb

Fig.7 DSC curves of PVB and PVB-Rhb（endo up）

Fig.8 DSC curves of PVB films and PVB-Rhb films with different mass fractions of PVB-Rhb （endo up）

Fig.9 Temperature dependence of the fluorescence lifetime curves for different fluorescence contents

Fig.10 Comparison of DSC and FLIM experimental results

Fig.11 Temperature dependence of the fluorescence lifetime curves for PVB/PVB-Rhb（2%） films of different thicknesses

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Probing the Glass Transition Temperature of Poly（vinyl butyral） Using Fluorescence Lifetime

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Figures/Tables 11

References 60

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