Katoueizaheh Elham, Rajabinejad Hossein, Rafferty Aran, Morris Michael A
School of Chemistry, CRANN and AMBER Research Centres, Trinity College Dublin Dublin 2 Ireland
RSC Adv. 2025 Sep 10;15(39):32746-32757. doi: 10.1039/d5ra03395k. eCollection 2025 Sep 5.
Polytetrafluoroethylene (PTFE) parts are normally consolidated under multi-tonne presses and sintered, but the separate roles of load and temperature on crystal development remain under-explored. Here, we molded PTFE powder under compressive loads (1.2, 1.8 and 2.4 kN) followed by sintering (320, 330 and 340 °C). The starting powder and molded films were characterised using X-Ray Diffraction (XRD), Fourier-Transform Infrared Spectroscopy (FTIR), Small-Angle X-Ray Scattering (SAXS), Dynamic Image Analysis (DIA) and Scanning Electron Microscopy (SEM). Raising the sintering temperature from 320 °C to 340 °C (at 1.8 kN) increased XRD-derived crystallinity from 63.5% to 71.8% and sharpened five hexagonal-phase reflections ((100)-(210)), while the and lattice parameters contracted by ∼0.3% and ∼1.1%, respectively, indicating tighter chain packing. SAXS revealed a concomitant 7% reduction in long-period spacing, and FTIR showed intensified CF and C-C bands, signifying enhanced chain alignment. In contrast, elevating the load from 1.2 kN to 2.4 kN at 320 °C trimmed bulk porosity from 33% to 25% without a statistically significant crystallinity change (63.0% → 64.8%). SEM cross-sections established that additional load mainly closes residual inter-particle voids rather than promoting crystal growth. Taken together, the data demonstrates that temperature is the primary driver of phase-IV hexagonal ordering, whereas load chiefly controls densification and has only a minor effect on ordering. This work, therefore, establishes a practical, low-pressure processing window 330 to 340 °C under ∼1.8 kN, which yields highly-ordered (≈72% crystalline), low-porosity (≈25%) PTFE films, providing a cost-effective route for manufacturing PTFE films and components.
聚四氟乙烯(PTFE)部件通常在多吨压力机下进行压制并烧结,但是载荷和温度在晶体生长过程中所起的各自作用仍未得到充分研究。在此,我们在压缩载荷(1.2、1.8和2.4 kN)下对PTFE粉末进行模压,随后进行烧结(320、330和340°C)。使用X射线衍射(XRD)、傅里叶变换红外光谱(FTIR)、小角X射线散射(SAXS)、动态图像分析(DIA)和扫描电子显微镜(SEM)对起始粉末和模压薄膜进行了表征。将烧结温度从320°C提高到340°C(在1.8 kN载荷下),XRD测定的结晶度从63.5%提高到71.8%,并使五个六方相反射峰((100)-(210))变尖锐,同时a和c晶格参数分别收缩了约0.3%和约1.1%,表明链堆积更紧密。SAXS显示长周期间距相应减小了7%,FTIR显示CF和C-C谱带增强,表明链排列增强。相比之下,在320°C下将载荷从1.2 kN提高到2.4 kN,总体孔隙率从33%降至25%,结晶度没有统计学上的显著变化(63.0%→64.8%)。SEM横截面表明,额外的载荷主要是封闭了颗粒间的残余空隙,而不是促进晶体生长。综合来看,数据表明温度是六方相IV有序化的主要驱动因素,而载荷主要控制致密化,对有序化的影响较小。因此,这项工作确定了一个实用的低压加工窗口,即330至340°C、约1.8 kN的载荷,可制备出高度有序(≈72%结晶)、低孔隙率(≈25%)的PTFE薄膜,为PTFE薄膜及部件的制造提供了一条经济高效的途径。