Morphological and structural development of poly(ether ether ketone) during mechanical pulverization
Morphological and structural development of poly(ether ether ketone) during mechanical pulverization
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DOI：
10.1002/app.26916
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发表时间：
2007-12
影响因子：
3
通讯作者：
Mei Liang;Canhui Lu;Yigang Huang;Changsheng Zhang
中科院分区：
文献类型：
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作者：
Mei Liang;Canhui Lu;Yigang Huang;Changsheng Zhang
采用自行研制的盘式球磨设备，在室温下制备了微米级聚醚醚酮（PEEK）粉体。通过SEM、WAXD、DSC、TGA和粘度计分析，研究了球磨过程中颗粒形态、结晶性能、热行为和粘均分子量的变化。SEM分析表明，磨盘碾磨首先通过磨盘间的挤压破坏了PEEK的原有结构，然后经过变形和尺寸减小的过程，生成细粉。PEEK的平均粒径仅在5个循环的盘磨后才减小到100 μm，并且在50个循环后达到小于50 μm。DSC分析表明，PEEK的结晶度随着球磨次数的增加而降低，与WAXD数据一致。经过50次球磨循环，PEEK的结晶度从46.2%下降到39.9%。玻璃化转变温度随着球磨次数的增加而沿着升高。还研究了球磨过程中的机械力化学效应。粘度计测试表明，分子量在磨浆前期下降较快，磨浆后期略有下降。盘磨技术是一种高效、清洁、环保的PEEK超细粉体制备方法。© 2007威利期刊公司应用聚合物科学杂志2007
Micron size particles of poly(ether ether ketone) (PEEK) were prepared by self-made pan-type milling equipment operated at ambient temperature. The changes of particle morphology, crystalline properties, thermal behavior, and viscosity-average molecular mass during milling were studied by SEM, WAXD, DSC, TGA, and viscosimetry analyses, respectively. SEM analysis indicated that pan-milling firstly destroyed the original structure of PEEK through squeezing in-between mill pans, then to produce fine powder undergoing the processes of deforming and size reduction. The average particle size of PEEK was reduced to 100 μm only after 5 cycles of pan-milling and reached less than 50 μm after 50 cycles. DSC analysis showed that crystallinity of PEEK decreased with the pan-milling cycles, agreed with WAXD data. The crystallinity of PEEK decreased from 46.2 to 39.9% of 50 pan-milling cycles was offered. The glass transition temperature increased slightly along with pan-milling cycles. Mechanochemical effects caused by pan-milling were also studied. Viscometer test exhibited that molecular weight dropped quickly at earlier pan-milling stage then decreased slightly during later pan-milling. Pan-milling technique is an efficient, clean, and environmental friendly method for preparing fine PEEK powder. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007