Accurate measurement of the localized degree of grafting using thermogravimetric analysis

IF 6.3 2区化学 Q1 POLYMER SCIENCE Polymer Degradation and Stability Pub Date : 2024-11-21 DOI:10.1016/j.polymdegradstab.2024.111087

Masaaki Omichi , Hiroyuki Hoshina , Hidenobu Morishima , Kunihiro Ohshima , Noriaki Seko

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Abstract

A method for accurately measuring the degree of grafting (DG) in a small area of several tens of square millimeters to several tens of square centimeters is proposed. This method employs thermogravimetric analysis to take advantage of the similarity in pyrolysis behavior of grafted materials with similar DGs. A pre-irradiation method is used for graft polymerization with an acrylic acid monomer to a cotton fibers substrate, and the proposed method is used to quantify the DG of the grafted material. Cryo-milling is used to homogenize the grafted material, and reference samples with known DGs (DG: 1.9 %–107.0 %) are prepared. Subsequently, localized DG is determined by measuring the pyrolysis behavior and comparing it to that of the reference samples. In experiments, the proposed method accurately predicts the DGs of test samples with a difference of <1.0 % from gravimetric measurements, especially at low DGs of 0 %–40.0 %. The proposed method can also detect the DG distribution of a cotton fiber substrate with a thickness of <1 mm. The proposed method is expected to be useful for detecting heterogeneous graft reactions and improving quality control of grafted materials in industrial applications.

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利用热重分析法精确测量局部接枝程度

提出了一种在几十平方毫米到几十平方厘米的小范围内精确测量接枝度（DG）的方法。该方法采用热重分析法，利用具有相似接枝度的接枝材料在热解行为上的相似性。采用预辐照法将丙烯酸单体接枝聚合到棉纤维基材上，并利用所提出的方法量化接枝材料的 DG。使用低温研磨技术均匀化接枝材料，并制备已知 DG 的参考样品（DG：1.9 %-107.0 %）。随后，通过测量热解行为并将其与参考样品的热解行为进行比较，确定局部 DG。在实验中，所提出的方法能准确预测测试样品的 DG，与重量测量值的差异仅为 1.0%，尤其是在 0%-40.0% 的低 DG 值下。该方法还能检测厚度为 1 毫米的棉纤维基材的 DG 分布。预计该方法将有助于检测异质接枝反应，并改善工业应用中接枝材料的质量控制。

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来源期刊

Polymer Degradation and Stability 化学-高分子科学

CiteScore

10.10

自引率

10.20%

发文量

325

审稿时长

23 days

期刊介绍： Polymer Degradation and Stability deals with the degradation reactions and their control which are a major preoccupation of practitioners of the many and diverse aspects of modern polymer technology. Deteriorative reactions occur during processing, when polymers are subjected to heat, oxygen and mechanical stress, and during the useful life of the materials when oxygen and sunlight are the most important degradative agencies. In more specialised applications, degradation may be induced by high energy radiation, ozone, atmospheric pollutants, mechanical stress, biological action, hydrolysis and many other influences. The mechanisms of these reactions and stabilisation processes must be understood if the technology and application of polymers are to continue to advance. The reporting of investigations of this kind is therefore a major function of this journal. However there are also new developments in polymer technology in which degradation processes find positive applications. For example, photodegradable plastics are now available, the recycling of polymeric products will become increasingly important, degradation and combustion studies are involved in the definition of the fire hazards which are associated with polymeric materials and the microelectronics industry is vitally dependent upon polymer degradation in the manufacture of its circuitry. Polymer properties may also be improved by processes like curing and grafting, the chemistry of which can be closely related to that which causes physical deterioration in other circumstances.