Development of polar phases in poly(vinylidene fluoride-co-hexafluoropropylene)/Expanded Graphite composites during 3-D printing as revealed by “operando” small and wide angle X-ray scattering

IF 4.5 2区化学 Q2 POLYMER SCIENCE

Polymer Pub Date : 2025-10-08 DOI:10.1016/j.polymer.2025.129198

Tiberio A. Ezquerra, Oscar Gálvez, Mari Cruz García-Gutiérrez, Marc Malfois, Aurora Nogales, Esther Rebollar, Igors Šics

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Abstract

Here we present a research work about the crystallization of poly(vinylidene fluoride-co-hexafluoropropylene) (PVDF-HFP) and of one PVDF-HFP composite with expanded graphite (EG) as nanoadditive during 3D printing Fused Filament Fabrication (FFF). Simultaneous Small and Wide Angle X-ray Scattering experiments (SAXS and WAXS) were performed “in situ” under “operando” conditions. The X-ray experiments clearly reveal the presence of a polar phase in the PVDF-HFP/EG while for PVDF-HFP its presence is not obvious. Complementary Fourier Transform Infrared Spectroscopy experiments corroborate the presence of the polar phase for both materials. For PVDF-HFP crystallization is faster at the interfaces (polymer-air and polymer-polymer) than in other points within a printed line, being the crystallinity lower at the interfaces. However, for the PVDF-HF composite, neither crystallization rate nor crystallinity is dependent on position. The effect of EG, acting as nucleating agent, has been discussed as being the reason for this behavior.

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“operando”小广角x射线散射揭示了聚偏氟乙烯-共六氟丙烯/膨胀石墨复合材料在3d打印过程中极性相的发展

本文研究了聚偏氟乙烯-共六氟丙烯（PVDF-HFP）和一种以膨胀石墨（EG）为纳米添加剂的PVDF-HFP复合材料在3D打印熔丝制造（FFF）中的结晶过程。同时在“operando”条件下进行了小角和广角x射线散射实验（SAXS和WAXS）。x射线实验清楚地显示PVDF-HFP/EG中存在极性相，而PVDF-HFP中极性相的存在并不明显。互补傅里叶变换红外光谱实验证实了两种材料的极性相的存在。PVDF-HFP的结晶在界面处（聚合物-空气和聚合物-聚合物）比在印刷线内的其他点要快，因为界面处的结晶度较低。然而，对于PVDF-HF复合材料，结晶速率和结晶度都不依赖于位置。讨论了EG作为成核剂的作用是造成这种行为的原因。

本文章由计算机程序翻译，如有差异，请以英文原文为准。

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来源期刊

Polymer 化学-高分子科学

CiteScore

7.90

自引率

8.70%

发文量

959

审稿时长

32 days

期刊介绍： Polymer is an interdisciplinary journal dedicated to publishing innovative and significant advances in Polymer Physics, Chemistry and Technology. We welcome submissions on polymer hybrids, nanocomposites, characterisation and self-assembly. Polymer also publishes work on the technological application of polymers in energy and optoelectronics. The main scope is covered but not limited to the following core areas: Polymer Materials Nanocomposites and hybrid nanomaterials Polymer blends, films, fibres, networks and porous materials Physical Characterization Characterisation, modelling and simulation* of molecular and materials properties in bulk, solution, and thin films Polymer Engineering Advanced multiscale processing methods Polymer Synthesis, Modification and Self-assembly Including designer polymer architectures, mechanisms and kinetics, and supramolecular polymerization Technological Applications Polymers for energy generation and storage Polymer membranes for separation technology Polymers for opto- and microelectronics.