ISSN 1008-5548

CN 37-1316/TU

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Curing behavior regulation and superhydrophobic construction of hyperbranched siloxane-modified PVDF fluorocarbon coatings

DUAN Guangbin1 ,WU Yutao2 ,LEI Xinjun2 ,LIU Kun2 ,XU Lushuo2 ,GENG Bing1

1. School of Materials Science and Engineering, University of Jinan, Jinan 250022, China;2. Pingnai New Materials Technology (Shandong) Co. , Ltd. , Heze 274300, China

Abstract

Objective Fluorocarbon coatings based on polyvinylidene fluoride (PVDF) are widely recognized for their long-term protection performance, but their inert backbone and multi-stage thermal evolution often lead to limited process controllability and unstable surface functions. Hyperbranched polysiloxane (HBP) provides multi-site interfacial regulation and low-surface-energy segments, offering a feasible approach to concentrating the thermal process and improving coating uniformity. This study aims to clarify how HBP reshapes the thermal pathway of PVDF coatings and construct a superhydrophobic surface through the gel-state deposition of MTMS-DEMS-SiO2 nanoparticles.

Methods HBP was synthesized from KH550 via hydrolysis/condensation reactions and subsequently incorporated into PVDF to prepare modified coatings, PVDF-0—PVDF-3. Fourier transform infrared spectroscopy (FTIR) and scanning electron microscopy coupled with energy-dispersive X-ray spectroscopy (SEM-EDS) were employed to evaluate the preservation of the PVDF structure and the distribution of silicon (Si) elements. The thermal curing behavior was analyzed using differential scanning calorimetry (DSC), supplemented with calculated conversion curves (α-T) and derivative curves (dα/dT-T) to quantify the evolution of the thermal process. Thermal stability was evaluated using thermogravimetric analysis and derivative thermogravimetry (TG-DTG). PVDF-4 was obtained by depositing MTMS-DEMS-SiO2 onto PVDF-3 in the gel state, followed by curing and contact-angle measurement.

Results and Discussion FTIR analysis indicated that PVDF characteristic peaks remained essentially unchanged after modification, while SEM-EDS confirmed effective and more uniform Si incorporation at the coating surface. DSC thermograms showed that PVDF-0 exhibited two peaks, while PVDF-3 changed to one dominant peak. Consistently, dα/dT-T displayed two rate peaks for PVDF-0 (75~95 ℃ and 125~135 ℃) but mainly a single low-temperature peak for PVDF-3, and α-T demonstrated earlier conversion of PVDF-3 at mid-low temperatures, indicating a "two-step to one-step" concentrating effect. TG-DTG showed Tonset decreases from 331 ℃ to 316 ℃ and Tmax shifts from 357. 55 ℃ to 347. 02 ℃ , while the 600 ℃ residue increased from 52. 23% to 53. 67%. Gel-state deposition of MTMS-DEMS-SiO2 yielded hierarchical roughness and increased the static water contact angle from 100°to 158°, achieving superhydrophobicity.

Conclusion In this study, HBP enables effective interfacial integration without altering PVDF’s main functional groups and concentrates the thermal process from dual-peak to single-peak behavior, which helps simplify the curing schedules. Gel-state MTMS-DEMS-SiO2 deposition further constructs hierarchical roughness, producing a superhydrophobic PVDF coating with 158°contact angle.

Keywords:hyperbranched siloxane; fluorocarbon coating; curing process; superhydrophobic surface

Get Citation:DUAN Guangbin, WU Yutao, LEI Xinjun, et al. Curing behavior regulation and superhydrophobic construction of hyperbranched siloxane-modified PVDF fluorocarbon coatings[J]. China Powder Science and Technology,2026,32(4):1−12.

Received: 2024-12-26, Revised: 2026-01-06, Online: 2026-01-21.

Funding:The research was supported by the National Natural Science Foundation of China (Grant No. 52272017), the Talent Introduction Project for Urgent Needs in Key Supporting Regions of Shandong Province, and Natural Science Foundation of Shandong Province (Grant No. ZR2023LFG004).

DOI:10.13732/j.issn.1008-5548.2026.04.017

CLC No:TB3;TQ63;TB44                      Type Code: A

Serial No:1008-5548(2026)04-0001-12