聚合物薄膜中聚合物薄膜的玻璃化转变温度的测量检测方案(白光干涉测厚)

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Film Metrology & More...For further information please contact us at info@thetametrisis.com or sales@thetametrisis.comThetaMetrisis @ 2014， www.thetametrisis.com ThetaMetrisis APPLICATION NOTE #013 Simultaneous Real-time monitoring of film thickness andrefractive index during thermal processing Goal： The determination of glass transition temperature of polymeric films through the real time monitoringof thickness and refractive index of the film during thermal processing. Means & Methods： An FR-Thermal VIS/NIR configured to operate in the 360-1000nm spectral range is used.The hot plate integrated on the tool， is controlled either manually or through the FR-Monitor software. In thepresent case the thickness and the refractive index (Cauchy model) of the film are monitored during theheating at a constant rate. The polymers investigated were poly(iso-butyl methacrylate) (PiBMA)， poly(n-propyl methacrylate) (PPMA) and poly(ethyl methacrylate) (PEMA) and their films are spin coated on siliconwafers. Prior to the measurements the samples have been Post Apply Baked at 145°℃ for 15min. Results： The heating rate is a 2-3℃/min and the polymeric film thickness and the refractive index aremonitored at 50 measurements / min and both parameters are plotted vs. temperature， figs. 1a-c. Clearly thepolymeric film thickness increase linearly with temperature at two temperature regimes. The intersect point ofthe extrapolated linear sections is defined as the grass transition temperature (Tg) of the polymer.The Tgvalues for these poly(alkyl methacrylate) films were found to be in agreement with the literature. The thickness increase rate is in good agreement with the reported values in the literature of thermalexpansion coefficient at each polymer’s "rubbery phase" i.e. at temperature values higher than Tg and in thesame order of magnitude with the reported values in the "glassy phase". Figure 1： Thermal treatment of methacrylate films and monitoring of film thickness and refractive index a) PiBMA， b)PBMA，c) PEMA. The calculated values of thermal expansion coefficients， depending on the temperature range，are ： (i)2.9-3.4*10° for TTg. These values are in agreement with the bibliography datafor these poly(alkyl methacrylates). Conclusions： The glass transmission temperature of polymeric films was measured with an FR-Basic equippedwith the FR-Thermal kit. In a similar way other thermal parameters of polymeric films can be also determinede.g. Degradation temperature of polymeric films. ( 1 N.Vourdas， G.Karadimos， D.Goustouridis， E.Gogolides， A.G.Boudouvis，J.-H.Tortai， K.Be l tsios，I.Raptis， J. Appl. Polym. Sci.， "Multi-wavelength i n terferometry and competing optical methods for the thermal probing of thin polymeric films" 200 6 ， 102，4764-4774 ) ( " Y. Diamant， S . Welner and D. K atz， J. P olymer， “Gl a ss transition tem p eratures of crosslinked poly (isobutyl methacrylate)" 1970， 11， 498-506， ) ( S. S. Rogers a n d L. M a ndelkern， J. Ph y s. Chem.， “Glass formation in p olymers. I. The gla s s transitions of poly(n-alkylmetacrylates)" 1957， 61，985-991 ) 4*J.E. Mark， “Physical Properties of Polymers Handbook"， Springer，2007 热处理过程中薄膜厚度和折射率的实时实时监测目的：通过热处理过程中对薄膜厚度和折射率的实时监测，确定聚合物薄膜的玻璃化转变温度。方法：使用配置为在360-1000nm光谱范围内工作的FR-热VIS/NIR。集成在工具上的热板，是手动或通过FR-Monitor控制的。 Ftware。在目前的情况下，薄膜的厚度和折射率（柯西模型）在恒定速率的加热过程中被监测。所研究的聚合物为聚异丁基甲烷 丙烯酸酯（PIBMA）、聚甲基丙烯酸正丙酯（PPMA）和聚甲基丙烯酸乙酯（PEMA）及其薄膜在硅片上自旋包覆。在测量之前，样品已被后置 在145°C下浸泡15分钟。结果：加热速率为2-3oC/min，聚合物膜厚度和折射率在50次测量/min时被监测，并绘制了两个参数与温度的关系图，无花果。1a-c. 显然，在两种温度条件下，聚合物膜厚度随温度呈线性增加。外推线性剖面的交点被定义为草的过渡温度。厚度增加率与文献中报道的每种聚合物的“橡胶相”热膨胀系数值吻合较好。当温度值高于T时 并在相同的数量级与报告的数值在“玻璃相”4。甲基丙烯酸酯薄膜的热处理以及薄膜厚度和折射率的监测a）PiBMA，b）PBMA，c）PEMA。 根据温度范围，热膨胀系数的计算值是：（i）对于T <Tg为2.9-3.4 * 10-4，并且（ii）对于T> Tg为6.4-6.7 * 10-4。 这些值与这些聚（甲基丙烯酸烷基酯）4的书目数据一致。结论：用装有FR-热试剂盒的FR-Basic测量了聚合物薄膜的玻璃透射温度。类似地，还可以确定聚合物薄膜的其他热参数例如：聚合物膜的降解温度。FR的工具基于白光反射光谱(Reports) 。准确同步的厚度测量及薄膜的折射率-一个广泛的多样化的应用范围广泛的光电特性的工具和整体解决方案，如:半导体、有机电子、聚合物、涂料和涂料、光伏、生物传感、化学传感...