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应用广角X-射线衍射(WAXD)来测定高聚物的结晶度可以分为相对法(CCI、ICI)与绝对法(HWM、CPRM、Ruland)两大类,但长期以来在文献上这些方法得出的结果往往差别很大,而且WAXD与其它的方法,如DSC、ρ、NMR、IR等往往也不相一致。本文就此两问题进行了系统的研究,不仅对WAXD与DSC、ρ测定结晶度的可靠性进行了讨论,更对WAXD的各种方法中,2θ应选的范围、是否应作校正、非晶散射如何扣除、相对法自身之间的关系、各种绝对法之间的关系、相对法与绝对法的关系等进行了仔细的研究。结论是:WAXD在可靠性与重复性方面优于DSC与ρ法,而且是其它方法的根据;绝对法优于相对法,各种绝对法有利有弊,而非晶散射的合理分离是最为关键的问题。
The wide-angle X-ray diffraction (WAXD) to determine the crystallinity of polymers can be divided into two categories: relative method (CCI, ICI) and absolute method (HWM, CPRM, Ruland) The results are often very different, and WAXD and other methods, such as DSC, ρ, NMR, IR, often not consistent. In this paper, a systematic study of these two issues, not only for WAXD and DSC, ρ determination of the reliability of the determination of the degree of crystallinity are discussed, more WAXD various methods, the 2θ should be selected range, should be corrected, amorphous scattering How to deduct, the relationship between relative law itself, the relationship between various absolute laws and the relationship between relative law and absolute law. The conclusion is: WAXD is superior to DSC and ρ in terms of reliability and repeatability, and is the basis of other methods; absolute method is better than relative method, all kinds of absolute method have both advantages and disadvantages, and the reasonable separation of amorphous scattering is the most crucial The problem.