无机粒子杂化聚酰亚胺(PI)薄膜具有优良的耐电晕特性,广泛用于变频电机中,文章首先用偶联剂处理过的超细氧化铝粉掺杂聚酰胺酸(PAA)制备了不同氧化铝含量的聚酰亚胺杂化膜。通过傅里叶变换红外光谱(FTIR)、X射线光电子能谱(XPS)、电感耦合等离子发射光谱(ICP)、重量法、热失重(TG/空气气氛)等测试方法对制备的不同Al₂O₃含量杂化聚酰亚胺薄膜的无机成分进行了定性和定量分析。结果表明:FTIR和XPS能很好地对杂化膜进行定性分析,FTIR主要对材料的结构进行分析从而推断出其可能的成分,而XPS则主要得到材料所含各元素信息,它具有操作简单,重复性好等优点;通过研究内层电子结合能及其氧化态的变化,XPS可以鉴别元素种类和价态、测定元素的相对含量。XPS和TG的实测值和理论值相差较大,相对标准偏差(RSD)很大,其中,XPS的RSD值大于5.0%,而TG的RSD值也都大于2.0%,只能对杂化膜进行半定量分析。而ICP和重量法的实测值和理论值相差较小且相对标准偏差(RSD)很小,它们的RSD值均小于1.0%,能进行精确的定量分析,其中重量法的实测值最接近理论值,但只能用于单一无机组分的分析;而ICP法最精确且可以对多无机组分的复合物进行分析,它有简便、快速、灵敏度高、准确性好、可多元素同时测定,且对环境污染小等优点。由上面的结论可以得到一种分析复合材料中的无机成分的方法:首先,用FTIR和XPS对复合材料进行定性分析;然后,以XPS半定量分析结果作为参考,用重量法(单一组分)和ICP法对复合材料进行精确的定量分析。

The inorganic particles hybrid polyimide films are newly emerging advanced materials with excellent corona-resistant and have been widely used in frequency control motor.The Al₂O₃/PI hybrid films with different Al₂O₃ contents were prepared by superfine aluminum power treated by coupling agent and polyamide acid (PAA).Qualitative analysis and quantitative analysis on the inorganic content to it were conducted using Fourier Transform Infrared Spectroscope (FTIR),X-ray photoelectron spectroscopy (XPS),Inductively coupled plasma spectrometry (ICP),Gravimetric method,Thermogravimetric Analysis (TG/air atmosphere).It was found that FTIR and XPS arE_good qualitative analysis methods.FTIR is used to inference possible components by analyzing the structure of material.The method has a lot of advantages such as easily operational,good repeatability,high accuracy and so on.XPS is mainly used to get information of elements contained in the material,it provides information about the core level binding energies and oxidation states of complexes.It can be used to identify the species and valence states of elements,measure the relative content of elements.The relative standard deviations (RSDs) of XPS and TG are too great to perform quantitative analysis,the RSDs of XPS are all above 5.0%,and TG’s RSDs are also above 2.0%.So they can be only used as semiquantitative analysis methods.On the contrary,ICP and Gravimetric method are two excellent quantitative analysis methods,their RSDs are all below 1.0％.Moreover Gravimetric method only can be used to analyze single inorganic constituent complex material,although its measured value is closest approach to theoretical value.ICP is the most accurate method and it can be used to analyze multi inorganic components in complex material,this method proved to be easily operational,rapid,highly sensitive,and accurate,and can be adopted as the method of determining many elements simultaneously.So a method was got to analysis of inorganic constituent in complex material from the conclusion upward.Firstly,components in complex material are defined by using FTIR and XPS as qualitative analysis methods and then using the result of XPS as a reference,exactly quantitative analysis of inorganic constituent in complex material was performed by using Gravimetric method and ICP.