CN110887854A - 应用二维x射线衍射检测聚丙烯腈纤维广义取向度的方法 - Google Patents

应用二维x射线衍射检测聚丙烯腈纤维广义取向度的方法 Download PDF

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CN110887854A
CN110887854A CN201811041121.5A CN201811041121A CN110887854A CN 110887854 A CN110887854 A CN 110887854A CN 201811041121 A CN201811041121 A CN 201811041121A CN 110887854 A CN110887854 A CN 110887854A
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高忠民
唐海通
高宇
李向山
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Jilin University
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Abstract

本发明提供了一种应用二维X射线衍射检测聚丙烯腈纤维广义取向度的方法，属于材料结晶结构分析检测技术领域。国内外应用的PAN纤维X射线法测量取向度的方法均是针对结晶相(100)衍射线进行的，但有明显的不完整性和不准确性。因此本发明提出了一种以二维衍射图谱为基础，选择特征衍射角，进行积分求取衍射强度‑方位角曲线，利用该曲线的半高峰宽计算得到结晶相取向度Ac,取向非晶相取向度Ao和非晶相取向度Aa，完整的表征了PAN纤维中结晶相、取向非晶相及非晶相中的取向状态，相比现有技术结果更加准确。

Description

应用二维X射线衍射检测聚丙烯腈纤维广义取向度的方法
技术领域
本发明属于材料结晶结构分析检测技术领域。
背景技术
聚丙烯腈纤维是制造优质碳纤维的前驱体，其结构特点对碳纤维的质量有重要影响。PAN纤维属于大分子链构象，在分子链内的原子为共价强键连接，而分子链间属于氢键及范德华力弱键作用。因此分子链的取向状态对聚丙烯腈(PAN)纤维原丝轴向强度与模量有重要影响，因此其中结晶相、取向非晶相及非晶相的沿纤维轴的取向行为是PAN纤维的关键性结构参数。至今国内外应用的PAN纤维X射线法测量取向度的方法均是针对结晶相(100)衍射线进行的，但有明显的不完整性和不准确性。
发明内容
本发明的目的在于在全面考虑PAN纤维中多类结晶类型对PAN纤维取向参数的贡献前提下创建全新的PAN纤维广义取向度表征技术。为此本发明提出了一种应用二维X射线衍射检测聚丙烯腈纤维广义取向度的方法，采用的技术方案具体如下：
1)应用二维X射线衍射仪测试聚丙烯腈纤维，获得二维衍射图谱，同时能够得到I(2θ，κ)曲线，即衍射强度-衍射角-方位角曲线；
2)针对结晶相，选择(100)晶面衍射角2θc＝16.9°，在衍射角2θc±Δ2θ范围内求曲线积分；针对取向非晶相，选择衍射角2θo＝25.2°，在衍射角2θo±Δ2θ范围内求曲线积分；分别获得I～κ曲线，即衍射强度-方位角曲线；Δ2θ为1°～5°；
3)对两条I～κ曲线分别计算半高峰宽，结晶相曲线半高宽为Hc，取向非晶相曲线半高宽为Ho，取向非晶相曲线的基线宽度为Ha＝180°；
4)按照以下公式计算得到结晶相取向度Ac,取向非晶相取向度Ao和非晶相取向度Aa；
Figure BDA0001792110530000011
Figure BDA0001792110530000012
Figure BDA0001792110530000013
本发明的有益效果：
本发明全面考虑了PAN纤维中多类结晶类型对PAN纤维取向参数，克服了现有技术只对结晶相的取向度进行检测造成的结构参数描述PAN纤维不准确、不全面的问题。
附图说明
图1实施例1聚丙烯腈纤维二维衍射图谱；
图2实施例1结晶相和取向非晶相的I～κ曲线。
具体实施方式
下面以具体实施例的方式对本发明技术方案做进一步解释和说明。
1)应用二维X射线衍射仪测试聚丙烯腈纤维，获得二维衍射图谱，同时能够得到I(2θ，κ)曲线，即衍射强度-衍射角-方位角曲线；
2)针对结晶相，选择(100)晶面衍射角2θc＝16.9°，在衍射角2θc±Δ2θ范围内求曲线积分；针对取向非晶相，选择衍射角2θo＝25.2°，在衍射角2θo±Δ2θ范围内求曲线积分；分别获得I～κ曲线，即衍射强度-方位角曲线；Δ2θ为1°～5°；
3)对两条I～κ曲线分别计算半高峰宽，结晶相曲线半高宽为Hc＝50.74°，取向非晶相曲线半高宽为Ho＝143.26°，取向非晶相曲线的基线宽度为Ha＝180°；
4)按照以下公式计算得到结晶相取向度Ac,取向非晶相取向度Ao和非晶相取向度Aa；
Figure BDA0001792110530000021
Figure BDA0001792110530000022
Figure BDA0001792110530000023

Claims (1)

1.应用二维X射线衍射检测聚丙烯腈纤维广义取向度的方法，其特征在于，所述的广义取向度包含三个参量，即结晶相取向度Ac,取向非晶相取向度Ao和非晶相取向度Aa；
检测的具体步骤如下：
1)应用二维X射线衍射仪测试聚丙烯腈纤维，获得二维衍射图谱，同时能够得到I(2θ，κ)曲线，即衍射强度-衍射角-方位角曲线；
2)针对结晶相，选择(100)晶面衍射角2θc＝16.9°，在衍射角2θc±Δ2θ范围内求曲线积分；针对取向非晶相，选择衍射角2θo＝25.2°，在衍射角2θo±Δ2θ范围内求曲线积分；分别获得I～κ曲线，即衍射强度-方位角曲线；Δ2θ为1°～5°；
3)对两条I～κ曲线分别计算半高峰宽，结晶相曲线半高宽为Hc，取向非晶相曲线半高宽为Ho，取向非晶相曲线的基线宽度为Ha＝180°；
4)按照以下公式计算得到结晶相取向度Ac,取向非晶相取向度Ao和非晶相取向度Aa；
Figure FDA0001792110520000011
Figure FDA0001792110520000012
Figure FDA0001792110520000013
CN201811041121.5A 2018-09-07 2018-09-07 应用二维x射线衍射检测聚丙烯腈纤维广义取向度的方法 Pending CN110887854A (zh)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103122495A (zh) * 2011-11-18 2013-05-29 东丽纤维研究所（中国）有限公司 一种改性共聚酯纤维及其制备方法和织物
CN107192729A (zh) * 2017-05-18 2017-09-22 吉林大学 聚丙烯腈纤维结构x射线衍射在线快速分析装置与方法

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103122495A (zh) * 2011-11-18 2013-05-29 东丽纤维研究所（中国）有限公司 一种改性共聚酯纤维及其制备方法和织物
CN107192729A (zh) * 2017-05-18 2017-09-22 吉林大学 聚丙烯腈纤维结构x射线衍射在线快速分析装置与方法

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
唐春红等: "湿法纺各阶段聚丙烯腈基原丝微结构的Ｘ射线衍射分析", 《化工新型材料》 *
徐翔等: "一种用X衍射测定PET纤维非晶取向度的简易方法", 《纺织学报》 *

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