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通过气相色谱-质谱联用热重分析法对超薄聚合物薄膜进行表征

Characterization of ultra-thin polymeric films by Gas chromatography-Mass spectrometry hyphenated to thermogravimetry.

作者信息

Gianotti Valentina, Antonioli Diego, Sparnacci Katia, Laus Michele, Giammaria Tommaso Jacopo, Ceresoli Monica, Ferrarese Lupi Federico, Seguini Gabriele, Perego Michele

机构信息

Dipartimento di Scienze e Innovazione Tecnologica (DISIT), Viale T. Michel 11, Università del Piemonte Orientale "A. Avogadro", INSTM, UdR Alessandria, 15121 Alessandria, Italy.

Dipartimento di Scienze e Innovazione Tecnologica (DISIT), Viale T. Michel 11, Università del Piemonte Orientale "A. Avogadro", INSTM, UdR Alessandria, 15121 Alessandria, Italy.

出版信息

J Chromatogr A. 2014 Nov 14;1368:204-10. doi: 10.1016/j.chroma.2014.09.073. Epub 2014 Oct 2.

DOI:10.1016/j.chroma.2014.09.073
PMID:25311490
Abstract

Polymeric materials are widely employed to build up tunable nanomasks for nano-patterning technologies. Ultrathin polymer layers are involved in this process. A Thermo Gravimetric Analysis-Mass Spectrometry (TGA-GC-MS) method was optimised, validated and successfully applied to investigate the thermal behavior of ultrathin poly(styrene-r-methylmethacrylate) random copolymer layers P(S-r-MMA) grafted to a silicon wafer surface. The interface between TGA and MS is highly versatile since many instrumental parameters (i.e. loop volumes, pulsed sampling frequencies, acquisition modalities, carrier gases, flow rates) can be easily tuned. Samples featuring substantial scale difference, i.e. bulk materials, thick films (few μm thickness), thin and ultrathin films (few nm thickness) can be analyzed without any instrumental modification or sample pretreatments. The TGA-GC-MS analysis was used to highlight subtle differences in samples featuring different thicknesses, in the 2-6 nm range, and subjected to various thermal treatments, thus indicating that this hyphenated technique could be successfully applied to the investigation of ultrathin polymer films.

摘要

聚合物材料被广泛用于构建用于纳米图案技术的可调谐纳米掩膜。超薄聚合物层参与了这一过程。一种热重分析-质谱联用(TGA-GC-MS)方法得到了优化、验证并成功应用于研究接枝到硅片表面的超薄聚(苯乙烯-无规-甲基丙烯酸甲酯)共聚物层P(S-r-MMA)的热行为。TGA和MS之间的接口具有高度通用性,因为许多仪器参数(即定量环体积、脉冲采样频率、采集方式、载气、流速)都可以轻松调整。对于具有显著尺寸差异的样品,即块状材料、厚膜(几微米厚)、薄膜和超薄薄膜(几纳米厚),无需任何仪器改装或样品预处理即可进行分析。TGA-GC-MS分析用于突出不同厚度(2-6纳米范围内)且经过各种热处理的样品之间的细微差异,从而表明这种联用技术可以成功应用于超薄聚合物薄膜的研究。

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