Determination of the degree of crystallinity of polyphenylene sulfide composited with crystalline and non-crystalline fillers by applying the direct derivation method

IF 5.2 3区 材料科学 Q2 CHEMISTRY, MULTIDISCIPLINARY
Hideo Toraya
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Abstract

A new procedure for determining the degree of crystallinity (DOC) has been recently proposed, and it has been verified using experimental and computer-generated powder diffractometry data [Toraya (2023). J. Appl. Cryst.56, 1751–1763]. As an application to real materials like engineering plastics, this procedure is here applied to the DOC determination of plate-like polyphenylene sulfide (PPS) samples, composited with crystalline and non-crystalline fillers. The coexistence of partially crystallized polymer with non-crystalline fillers in target materials makes it difficult to separate the non-crystalline part of the partially crystallized polymer. This problem is here solved by the inverse application of the direct derivation (DD) method for quantitative phase analysis (QPA). The intensity–composition (IC) formula used in the DD method can derive the weight fractions of the individual components from just the total sums of observed intensities and the chemical composition data for these components [Toraya (2016). J. Appl. Cryst.49, 1508–1516]. For the present purpose, the IC formula has been inversely applied to calculate the relative intensity ratios of individual components under the assumption that the chemical compositions and weight fractions of the respective components are known. The total halo intensity could then be separated into the non-crystalline part of the polymer and the non-crystalline filler. Analyzed results of PPS composites in four different DOCs are reported.

Abstract Image

采用直接推导法测定与结晶和非结晶填料复合的聚苯硫醚的结晶度
最近提出了一种测定结晶度 (DOC) 的新程序,并通过实验和计算机生成的粉末衍射数据对其进行了验证 [Toraya (2023)。 J. Appl. Cryst. 56, 1751-1763]。作为对工程塑料等实际材料的应用,本论文将这一程序应用于板状聚苯硫醚 (PPS) 样品的 DOC 测定,该样品由结晶和非晶填料组成。由于目标材料中部分结晶聚合物与非结晶填料共存,因此很难将部分结晶聚合物中的非结晶部分分离出来。本文通过将直接推导 (DD) 方法反向应用于定量相分析 (QPA) 来解决这一问题。DD 方法中使用的强度-成分(IC)公式可以仅从观测到的强度总和以及这些成分的化学成分数据中推导出各个成分的重量分数[Toraya (2016)。 J. Appl. Cryst. 49, 1508-1516]。为此,在已知各成分的化学成分和重量分数的前提下,反向应用 IC 公式计算各成分的相对强度比。这样就可以将总的光晕强度分为聚合物的非结晶部分和非结晶填料。报告了四种不同 DOC 中 PPS 复合材料的分析结果。
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来源期刊
Journal of Applied Crystallography
Journal of Applied Crystallography CHEMISTRY, MULTIDISCIPLINARYCRYSTALLOGRAPH-CRYSTALLOGRAPHY
CiteScore
7.80
自引率
3.30%
发文量
178
期刊介绍: Many research topics in condensed matter research, materials science and the life sciences make use of crystallographic methods to study crystalline and non-crystalline matter with neutrons, X-rays and electrons. Articles published in the Journal of Applied Crystallography focus on these methods and their use in identifying structural and diffusion-controlled phase transformations, structure-property relationships, structural changes of defects, interfaces and surfaces, etc. Developments of instrumentation and crystallographic apparatus, theory and interpretation, numerical analysis and other related subjects are also covered. The journal is the primary place where crystallographic computer program information is published.
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