CN111307804A - 金相显微镜测量聚丙烯腈预氧丝及碳纤维皮芯结构的方法 - Google Patents
金相显微镜测量聚丙烯腈预氧丝及碳纤维皮芯结构的方法 Download PDFInfo
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Abstract
本发明涉及聚丙烯腈碳纤维检测技术领域，具体涉及一种金相显微镜测量聚丙烯腈预氧丝及碳纤维皮芯结构的方法，解决聚丙烯腈碳纤维生产过程中聚丙烯腈预氧丝均质氧化评价手段缺乏的技术问题，包括下列步骤：包括聚丙烯腈预氧丝及碳纤维样品二次树脂包埋、树脂包埋样品的研磨抛光和聚丙烯腈预氧丝及碳纤维样品截面金相镜检观测。本发明可对整束聚丙烯腈预氧丝及碳纤维中每根单丝皮芯结构进行分析，信息全面。本发明针对聚丙烯腈预氧丝及碳纤维皮芯结构进行原位无损伤检测，成像清晰，信息真实。
Description
技术领域
本发明属于聚丙烯腈碳纤维检测技术领域，具体涉及一种金相显微镜测量聚丙烯腈预氧丝及碳纤维皮芯结构的方法。
背景技术
预氧化工艺是聚丙烯腈基碳纤维生产流程中一个重要步骤。在预氧化阶段发生双扩散：在浓差推动作用下，氧由纤维皮层向纤维芯部进行扩散；纤维芯部热解形成的小分子及降解反应副产物由纤维芯部向纤维皮层扩散。预氧化反应使聚丙烯腈线型分子链转变为耐热的梯形结构，同时在纤维皮层形成阻止氧向纤维芯部扩散的屏障，使氧沿纤维径向呈梯度分布，从而形成了皮芯结构，在后续碳化或石墨化过程中，聚丙烯腈预氧丝皮芯结构进一步发育并遗传给碳纤维，显著制约了碳纤维拉伸强度的提高。因此，消除预氧化过程形成的皮芯结构，调控纤维均质预氧化水平，是提高碳纤维拉伸强度和拉伸模量的重要技术途径。
申请号为201710699349.2的专利中公开了一种减弱碳纤维皮芯结构的设备和热处理方法。申请号为201010283935.7的专利中公开了一种利用拉曼光谱测试碳纤维皮芯结构的定量方法。申请号为201210253799.6的专利公开了一种碳纤维预氧丝皮芯结构的测定方法。中国科学院山西煤炭化学研究所公开了一种聚丙烯腈预氧化纤维皮芯结构的检测方法（专利申请号201611114005.2）。该方法将预氧化纤维短丝浸渍在硫酸溶液中刻蚀，再利用扫描电镜测量纤维及芯部直径，从而确定芯部所占比例。
这些测量聚丙烯腈预氧丝皮芯结构的方法具有局限性。拉曼光谱精密仪器的使用，限制了方法的普及；强酸处理预氧丝反应完全与否显著影响结果，且酸溶处理后的预氧丝轴向呈曲屈状态，用扫描电镜很难找到一个正视平面。另外，加热硫酸处理样品，存在安全隐患。因此，聚丙烯腈碳纤维生产过程需要一种原位无损伤检测聚丙烯腈预氧丝及碳纤维皮芯结构的方法。
发明内容
为了克服现有技术的不足，解决聚丙烯腈碳纤维生产过程中聚丙烯腈预氧丝均质氧化评价手段缺乏的技术问题，本发明提供一种金相显微镜测量聚丙烯腈预氧丝及碳纤维皮芯结构的方法。
本发明的设计构思：由于聚丙烯腈预氧丝和碳纤维皮层和芯部结构差异，在光学显微镜下呈现的光学活性明显不同，通过树脂包埋样品的研磨抛光技术制备光学分析试样，利用纤维皮层和芯部结构对金相显微镜偏振光响应差异，可以测定聚丙烯腈预氧丝和碳纤维皮芯结构。
本发明通过以下技术方案予以实现。
1、金相显微镜测量聚丙烯腈预氧丝及碳纤维皮芯结构的方法，其特征在于包括以下步骤：
S1、聚丙烯腈预氧丝及碳纤维样品二次树脂包埋，包括以下步骤：
S11、第一次树脂包埋：将聚丙烯腈预氧丝和碳纤维样品缠绕在不锈钢制样框上，控制张力使聚丙烯腈预氧丝和碳纤维样品在制样框上恰好拉直，将制样框浸入由环氧树脂、固化剂和丙酮组成的胶液中，浸胶时间为5～30min，取出制样框，擦除多余胶液后在烘箱中固化60～90min，完成聚丙烯腈预氧丝及碳纤维样品第一次树脂包埋；
S12、第二次树脂包埋：在橡胶模具中，使用冷镶嵌液体树脂对步骤S1中第一次树脂包埋处理后的聚丙烯腈预氧丝及碳纤维样品进行冷镶嵌，使聚丙烯腈预氧丝及碳纤维样品垂直固定于固化树脂中，剪去多余丝束，制得第二次树脂包埋的聚丙烯腈预氧丝和碳纤维样品；
S2、树脂包埋样品的研磨抛光：
首先，将步骤S12二次树脂包埋后的聚丙烯腈预氧丝和碳纤维样品垂直于轴向的平面，依次采用无水砂纸研磨、镜检观察、流动水清洗、超声清洗步骤处理，去掉聚丙烯腈预氧丝和碳纤维样品表面残留的砂粒；其次，由粗到细依次采用不同粒径的金刚石研磨膏依次在帆布和红色丝绒上对聚丙烯腈预氧丝和碳纤维样品抛光；再次，采用0.05微米氧化铝电极抛光粉在黑色呢绒上对聚丙烯腈预氧丝和碳纤维样品进行抛光，直至镜检观察到上一道工序抛光划痕被完全抛光除去；最后，通过流动清水清洗和抛光布擦除样品表面残留的抛光粉，干燥后得到适用于金相显微镜观察的聚丙烯腈预氧丝和碳纤维样品；
S3、聚丙烯腈预氧丝及碳纤维样品截面金相镜检观测：
将步骤S2制备的聚丙烯腈预氧丝和碳纤维样品放置于金相显微镜下，由低倍至高倍依次转换物镜，调整起偏镜、检偏镜和补偿镜片，调节孔径光阑、亮度和视场光阑按键，选取能够清晰反映样品截面形貌的区域进行观察，利用金相显微镜的标尺标定出聚丙烯腈预氧丝和碳纤维样品的直径和芯部直径。
与现有技术相比本发明的有益效果为：
(1) 、原位无损伤检测聚丙烯腈预氧丝及碳纤维皮芯结构，为聚丙烯腈碳纤维生产过程监测和工艺调整提供依据；
(2) 、本发明可对整束聚丙烯腈预氧丝及碳纤维中每根单丝皮芯结构进行分析，信息全面；
(3) 、本发明针对聚丙烯腈预氧丝及碳纤维皮芯结构进行原位无损伤检测，成像清晰，信息真实。
具体实施方式
以下实施例用于说明本发明，但不用来限制本发明的范围。若未特别指明，实施例均按照常规实验条件。另外，对于本领域技术人员而言，在不偏离本发明的实质和范围的前提下，对这些实施方案中的物料成分和用量进行的各种修改或改进，均属于本发明要求保护的范围。
实施例一
S1、选取规格为3k（3k代表3000根单丝）聚丙烯腈预氧丝样品进行二次树脂包埋。将聚丙烯腈预氧丝样品缠绕在不锈钢制样框上，控制张力使样品在制样框上刚好拉直，将制样框浸入由6101环氧树脂、三乙烯四胺固化剂和丙酮构成的胶液中浸胶约20min，取出制样框并擦除多余胶液、在烘箱中固化60～90min，完成聚丙烯腈预氧丝样品第一次树脂包埋。在橡胶模具中,使用冷镶嵌液体树脂将一次树脂包埋的聚丙烯腈预氧丝样品进行冷镶嵌，使样品垂直固定于固化树脂中，剪去多余丝束，制得二次树脂包埋的聚丙烯腈预氧丝样品。
S2、二次树脂包埋样品进行研磨抛光。将二次树脂包埋的聚丙烯腈预氧丝样品垂直于纤维轴向的平面依次采用无水砂纸研磨、镜检观察、流动水清洗、超声清洗等步骤处理，去掉表面残留的砂粒，再依次用7微米、2.5微米、0.5微米不同粒径的金刚石研磨膏，以及0.05微米氧化铝电极抛光粉，分别在帆布、红色丝绒和黑色呢绒上进行抛光，直至镜检观察到上一道工序抛光划痕被完全抛光除去，通过流动清水清洗和抛光布擦除样品表面残留的抛光粉，干燥后得到适用于金相显微镜观察的样品。
S3、聚丙烯腈预氧丝样品截面金相镜检。由低倍至高倍依次转换物镜，调整起偏镜、检偏镜和补偿镜片，调节孔径光阑、亮度和视场光阑按键，选取清晰反映样品截面形貌的区域进行观察，利用显微镜的标尺标定出聚丙烯腈预氧丝直径和芯部直径。
实施例二
S1、选取规格为12k（12k代表12000根单丝）聚丙烯腈碳纤维样品进行二次树脂包埋。将聚丙烯腈碳纤维样品缠绕在不锈钢制样框上，控制张力使样品在制样框上刚好拉直，将制样框浸入由双酚A二缩水甘油醚、甲基四氢邻苯二甲酸酐固化剂和二甲基苄胺构成的胶液中浸胶约20min，取出制样框并擦除多余胶液、在烘箱中固化60～90min，完成聚丙烯腈碳纤维样品第一次树脂包埋。在橡胶模具中,使用冷镶嵌液体树脂将一次树脂包埋的聚丙烯腈碳纤维样品进行冷镶嵌,使样品垂直固定于固化树脂中,剪去多余丝束，制得二次树脂包埋的聚丙烯腈碳纤维样品。
S2、二次树脂包埋样品进行研磨抛光。将二次树脂包埋的聚丙烯腈碳纤维样品垂直于纤维轴向的平面依次采用无水砂纸研磨、镜检观察、流动水清洗、超声清洗等步骤处理，去掉表面残留的砂粒，再依次用7微米、2.5微米、0.5微米不同粒径的金刚石研磨膏，以及0.05微米氧化铝电极抛光粉，分别在帆布、红色丝绒和黑色呢绒上进行抛光，直至镜检观察到上一道工序抛光划痕被完全抛光除去，通过流动清水清洗和抛光布擦除样品表面残留的抛光粉，干燥后得到适用于金相显微镜观察的样品。
S3、聚丙烯腈碳纤维样品截面金相镜检。由低倍至高倍依次转换物镜，调整起偏镜、检偏镜和补偿镜片，调节孔径光阑、亮度和视场光阑按键，选取清晰反映样品截面形貌的区域进行观察，利用显微镜的标尺标定出聚丙烯腈碳纤维直径和芯部直径。
实施例三
S1、选取规格为6k（6k代表6000根单丝）高强高模碳纤维(也称石墨纤维)样品进行二次树脂包埋。将石墨纤维样品缠绕在不锈钢制样框上，控制张力使样品在制样框上刚好拉直，将制样框浸入由双酚A二缩水甘油醚、甲基四氢邻苯二甲酸酐固化剂和二甲基苄胺构成的胶液中浸胶约25min，取出制样框并擦除多余胶液、在烘箱中固化60～90min，完成聚丙烯腈碳纤维样品第一次树脂包埋。在橡胶模具中，使用冷镶嵌液体树脂将一次树脂包埋的石墨纤维样品进行冷镶嵌，使样品垂直固定于固化树脂中，剪去多余丝束，制得二次树脂包埋的石墨纤维样品。
S2、二次树脂包埋样品进行研磨抛光。将二次树脂包埋的石墨纤维样品垂直于纤维轴向的平面依次采用无水砂纸研磨、镜检观察、流动水清洗、超声清洗等步骤处理，去掉表面残留的砂粒，再依次用7微米、2.5微米、0.5微米不同粒径的金刚石研磨膏，以及0.05微米氧化铝电极抛光粉，分别在帆布、红色丝绒和黑色呢绒上进行抛光，直至镜检观察到上一道工序抛光划痕被完全抛光除去，通过流动清水清洗和抛光布擦除样品表面残留的抛光粉，干燥后得到适用于金相显微镜观察的样品。
S3、聚丙烯腈碳纤维样品截面金相镜检。由低倍至高倍依次转换物镜，调整起偏镜、检偏镜和补偿镜片，调节孔径光阑、亮度和视场光阑按键，选取清晰反映样品截面形貌的区域进行观察，利用显微镜的标尺标定出石墨纤维直径和芯部直径。
以上所述，仅为本发明的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉技术领域的技术人员在本发明揭露的技术范围内，可轻易想到的变化或替换，都应涵盖在本发明的保护范围之内。因此，本发明的保护范围应以所述权利要求的保护范围为准。
Claims (1)
1.金相显微镜测量聚丙烯腈预氧丝及碳纤维皮芯结构的方法，其特征在于包括以下步骤：
S1、聚丙烯腈预氧丝及碳纤维样品二次树脂包埋，包括以下步骤：
S11、第一次树脂包埋：将聚丙烯腈预氧丝和碳纤维样品缠绕在不锈钢制样框上，控制张力使聚丙烯腈预氧丝和碳纤维样品在制样框上恰好拉直，将制样框浸入由环氧树脂、固化剂和丙酮组成的胶液中，浸胶时间为5～30min，取出制样框，擦除多余胶液后在烘箱中固化60～90min，完成聚丙烯腈预氧丝及碳纤维样品第一次树脂包埋；
S12、第二次树脂包埋：在橡胶模具中，使用冷镶嵌液体树脂对步骤S1中第一次树脂包埋处理后的聚丙烯腈预氧丝及碳纤维样品进行冷镶嵌，使聚丙烯腈预氧丝及碳纤维样品垂直固定于固化树脂中，剪去多余丝束，制得第二次树脂包埋的聚丙烯腈预氧丝和碳纤维样品；
S2、树脂包埋样品的研磨抛光：
首先，将步骤S12二次树脂包埋后的聚丙烯腈预氧丝和碳纤维样品垂直于轴向的平面，依次采用无水砂纸研磨、镜检观察、流动水清洗、超声清洗步骤处理，去掉聚丙烯腈预氧丝和碳纤维样品表面残留的砂粒；其次，由粗到细依次采用不同粒径的金刚石研磨膏依次在帆布和红色丝绒上对聚丙烯腈预氧丝和碳纤维样品抛光；再次，采用0.05微米氧化铝电极抛光粉在黑色呢绒上对聚丙烯腈预氧丝和碳纤维样品进行抛光，直至镜检观察到上一道工序抛光划痕被完全抛光除去；最后，通过流动清水清洗和抛光布擦除样品表面残留的抛光粉，干燥后得到适用于金相显微镜观察的聚丙烯腈预氧丝和碳纤维样品；
S3、聚丙烯腈预氧丝及碳纤维样品截面金相镜检观测：
将步骤S2制备的聚丙烯腈预氧丝和碳纤维样品放置于金相显微镜下，由低倍至高倍依次转换物镜，调整起偏镜、检偏镜和补偿镜片，调节孔径光阑、亮度和视场光阑按键，选取能够清晰反映样品截面形貌的区域进行观察，利用金相显微镜的标尺标定出聚丙烯腈预氧丝和碳纤维样品的直径和芯部直径。
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