芳纶纤维增强可溶性聚芳醚复合材料的制备技术、界面表征及性能研究
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摘要
本论文工作系国家自然科学基金(项目编号50743012)和辽宁省新世纪优秀人才(项目编号RC2005-14)的部分研究工作内容。论文中选用耐热等级最高的可溶性聚芳醚树脂—聚芳醚砜酮(PPESK)开展连续芳纶纤维增强热塑性树脂基复合材料缠绕成型工艺过程的纤维浸渍、制备方法、界面结构表征及其与性能关系的研究工作。针对芳纶纤维表面缺乏活性基团、表面光滑以及表面能低等问题,采用射频低温等离子体对芳纶纤维表面进行改性,对复合材料界面粘接性能进行优化设计。另外,对等离子体处理纤维表面的退化效应进行了初步探讨。
论文中选用目前应用最广和性能最好的有机芳纶纤维(Twaron和Armos)作为复合材料的增强相。采用氧气等离子体处理方法对芳纶纤维表面进行改性,利用溶液预浸渍工艺和高温模压成型技术制备了等离子体处理前后的芳纶纤维/PPESK树脂基复合材料。采用红外光谱(FTIR)、X-射线光电子能谱(XPS)、扫描电子显微镜(SEM)、原子力显微镜(AFM)以及动态接触角分析(DCAA)等方法研究了等离子体处理前后的芳纶纤维表面化学结构、元素组成、表面形貌、表面粗糙度以及表面浸润性能的变化。通过测试复合材料的层间剪切强度(ILSS)来表征复合材料的界面粘结性能。并对复合材料的吸水率进行测定来间接反映复合材料的界面粘结情况。通过对复合材料界面破坏形貌进行扫描观察,从而进一步分析复合材料的界面粘结机理。
本文首先考察了氧气等离子体处理对Twaron纤维表面及其复合材料界面性能的影响。结果表明:经过氧气等离子体处理之后,Twaron纤维表面引入了新的含氧官能团-COO-结构,表面粗糙度增加,表面浸润性能得到明显地改善。在等离子体处理功率为200W、处理时间为15min时,Twaron纤维/PPESK复合材料的层间剪切强度由未处理时的39.2MPa增加到52.0MPa,提高了32.6%。
其次,通过对等离子体处理时间与放电功率对Armos纤维表面状态及其复合材料的影响研究发现:氧气等离子体在Armos纤维表面引入了大量的含氧基团,同时对Armos纤维表面产生了明显的刻蚀作用,表面浸润性能得到相应地改善。在等离子体处理功率为200W、处理时间为10min时,Armos纤维/PPESK复合材料的层间剪切强度由未处理时的59.5MPa增加到68.8MPa,提高了15.6%。经等离子体处理之后,Armos纤维/PPESK复合材料的吸水率也表现出明显下降的趋势。但较长时间和较大功率的处理条件均会造成纤维表面剥离与消熔,纤维表面损伤严重,使得纤维表面极性官能团减少,表面粗糙度下降,浸润性不好,最终导致了Armos纤维/PPESK复合材料的界面粘结性能下降。
另外,通过对比等离子处理前后的芳纶纤维/PPESK复合材料层间剪切破坏断面形貌图发现,未处理时的复合材料断面处纤维表面光滑,粘附着少量的树脂,复合材料的破坏模式主要是界面破坏,而经过等离子体处理之后的复合材料断面处纤维表面粗糙并粘附着大量的树脂,此时的复合材料破坏模式由未处理时的界面破坏逐渐转变为基体或纤维本体的破坏。通过对复合材料界面结构与性能的关系分析发现,纤维与树脂基体间的化学键接和机械嵌合作用均有利于提高复合材料的界面粘结性能。
最后,考察了等离子体处理芳纶纤维的时效性问题。将等离子体处理后的芳纶纤维在空气中放置10天左右,发现纤维表面的化学组成和浸润性能随着储存时间延长发生明显的退化效应。而在时效的过程中,纤维表面形貌和粗糙度的变化不大。这可能与等离子体处理之后的纤维表面极性基团发生重排、翻转有关。另外,芳纶/PPESK复合材料的界面粘结强度随着储存时间的延长也是呈明显下降的趋势。由此可见,纤维表面化学状态的退化是造成其复合材料界面粘结性能下降的主导因素。
This work was financially supported by National Natural Science Foundation of China (No. 50743012) and Liaoning Excellent Talents in University (No. RC2005-14). One kind of novel thermoplastic resin with excellent thermal resistance and solubility-Poly (phthalazinone ether sulfone ketone)(PPESK) was chosen as resin matrix in composite system in our paper. The fiber soakage, preparation method, interfacial structure characteriztion and properties relationship during twisting and molding procedure of continuous aramid fibers reinforced PPESK composite were investigated. Due to the problems of fiber surface with few polar functional groups, smooth surface and low surface energy, low temperature plasma treatment on fiber surface modification was used. The composite interfacial adhesion was optimized design. In addition, the aging behavior of plasma treatment on fiber surface was at the primary stage discussed.
In our work, two kinds of organic aramid fibers including Twaron and Armos were modified by oxygen plasma treatment. The fibers reinforced PPESK composite before and after plasma treatment were prepared through solution impregnating process and high temperature molding technique. The changes of fiber surface chemical structure, element composition, surface morphology, surface roughness and surface wettability before and after plasma treatment were characterized by FT-IR spectra, X-ray photoelectron spectroscopy (XPS), scanning electronic microscopy (SEM), atomic force microscopy (AFM) and dynamic contact angle analysis (DCAA) system, respectively. The composite interfacial adhesion property was evaluated by interlaminar shear strength (ILSS), and indirectly illustrated by the water absorption measurements and composite fracture mechanism was analyzed by the morphology of interlaminar shear ruptures of composite observed by SEM.
The effects of oxygen plasma treatment on Twaron aramid fiber surface and its composite interfacial properties were first studied in this paper. The results showed a new oxygen-containing functional group -COO- was introduced onto the fiber surface, the fiber surface roughness increased and the fiber surface wettability was improved obviously after oxygen plasma treatment. Composite interlaminar shear strength increased from 39.2MPa for untreated sample to 52.0MPa for plasma treated for 15min under discharge power at 200 W, with an increase of 32.6%.
Secondly, the influence of plasma treatment condition such as time and discharge power on Armos fiber surface and its composite interfacial properties were studied. It was found that oxygen plasma could introduce a lot of oxygen-containing functional groups onto the fiber surface, the fiber surface was etched obviously and the fiber surface wettability was improved consequently. Composite interlaminar shear strength increased from 59.5MPa for untreated sample to 68.8MPa for plasma treated for 10min under discharge power at 200 W, with an increase of 15.6%. The water absorption of composite decreasing also indirectly showed that oxygen plasma treatment improved composite interfacial adhesion. However, long time and large discharge power would make the fiber surface melting. Then, the fiber surface polar functional group decreased, surface roughness declined and surface wettability degraded. Finally, the composite interfacial properties turned to be weak.
In addition, compared with the morphology of composite interlaminar shear ruptures before and after plasma treatment, it was found that the fibers were smooth with low amount of resin adhered to surface for the untreated specimen, the rupture took place near the interface between the fiber and matrix; However, a large proportion of fibers stuck tightly to matrix, the primary failure mode varied from interface failure to matrix or fiber failure for the oxygen plasma-treated specimen. It suggested that the interfacial bond strengths between the fiber and the matrix were well improved by oxygen plasma treatment. The relationship between the fiber surface characteristics and composite interfacial properties indicated that both the chemical bonding between the fiber and the matrix in composite system and the mechanical interaction contributed for increasing composite interfacial properties.
Finally, the aging behavior of plasma-treated fiber surface was studied. The fiber surface properties such as polar functional groups, surface morphology, surface roughness and surface wettability as a function of storage time in air after plasma treatment were measured. The fiber surface aging behavior could be detected obviously in chemical composition and surface wettability, whereas the surface morphology and roughness remained nearly stable after storing in air as long as 10 days after oxygen plasma treatment. The polar functional groups on fiber surface reorientated or reversaled may be responsible for the weak interfacial strength between the fiber and the matrix in composite system.
论文中选用目前应用最广和性能最好的有机芳纶纤维(Twaron和Armos)作为复合材料的增强相。采用氧气等离子体处理方法对芳纶纤维表面进行改性,利用溶液预浸渍工艺和高温模压成型技术制备了等离子体处理前后的芳纶纤维/PPESK树脂基复合材料。采用红外光谱(FTIR)、X-射线光电子能谱(XPS)、扫描电子显微镜(SEM)、原子力显微镜(AFM)以及动态接触角分析(DCAA)等方法研究了等离子体处理前后的芳纶纤维表面化学结构、元素组成、表面形貌、表面粗糙度以及表面浸润性能的变化。通过测试复合材料的层间剪切强度(ILSS)来表征复合材料的界面粘结性能。并对复合材料的吸水率进行测定来间接反映复合材料的界面粘结情况。通过对复合材料界面破坏形貌进行扫描观察,从而进一步分析复合材料的界面粘结机理。
本文首先考察了氧气等离子体处理对Twaron纤维表面及其复合材料界面性能的影响。结果表明:经过氧气等离子体处理之后,Twaron纤维表面引入了新的含氧官能团-COO-结构,表面粗糙度增加,表面浸润性能得到明显地改善。在等离子体处理功率为200W、处理时间为15min时,Twaron纤维/PPESK复合材料的层间剪切强度由未处理时的39.2MPa增加到52.0MPa,提高了32.6%。
其次,通过对等离子体处理时间与放电功率对Armos纤维表面状态及其复合材料的影响研究发现:氧气等离子体在Armos纤维表面引入了大量的含氧基团,同时对Armos纤维表面产生了明显的刻蚀作用,表面浸润性能得到相应地改善。在等离子体处理功率为200W、处理时间为10min时,Armos纤维/PPESK复合材料的层间剪切强度由未处理时的59.5MPa增加到68.8MPa,提高了15.6%。经等离子体处理之后,Armos纤维/PPESK复合材料的吸水率也表现出明显下降的趋势。但较长时间和较大功率的处理条件均会造成纤维表面剥离与消熔,纤维表面损伤严重,使得纤维表面极性官能团减少,表面粗糙度下降,浸润性不好,最终导致了Armos纤维/PPESK复合材料的界面粘结性能下降。
另外,通过对比等离子处理前后的芳纶纤维/PPESK复合材料层间剪切破坏断面形貌图发现,未处理时的复合材料断面处纤维表面光滑,粘附着少量的树脂,复合材料的破坏模式主要是界面破坏,而经过等离子体处理之后的复合材料断面处纤维表面粗糙并粘附着大量的树脂,此时的复合材料破坏模式由未处理时的界面破坏逐渐转变为基体或纤维本体的破坏。通过对复合材料界面结构与性能的关系分析发现,纤维与树脂基体间的化学键接和机械嵌合作用均有利于提高复合材料的界面粘结性能。
最后,考察了等离子体处理芳纶纤维的时效性问题。将等离子体处理后的芳纶纤维在空气中放置10天左右,发现纤维表面的化学组成和浸润性能随着储存时间延长发生明显的退化效应。而在时效的过程中,纤维表面形貌和粗糙度的变化不大。这可能与等离子体处理之后的纤维表面极性基团发生重排、翻转有关。另外,芳纶/PPESK复合材料的界面粘结强度随着储存时间的延长也是呈明显下降的趋势。由此可见,纤维表面化学状态的退化是造成其复合材料界面粘结性能下降的主导因素。
This work was financially supported by National Natural Science Foundation of China (No. 50743012) and Liaoning Excellent Talents in University (No. RC2005-14). One kind of novel thermoplastic resin with excellent thermal resistance and solubility-Poly (phthalazinone ether sulfone ketone)(PPESK) was chosen as resin matrix in composite system in our paper. The fiber soakage, preparation method, interfacial structure characteriztion and properties relationship during twisting and molding procedure of continuous aramid fibers reinforced PPESK composite were investigated. Due to the problems of fiber surface with few polar functional groups, smooth surface and low surface energy, low temperature plasma treatment on fiber surface modification was used. The composite interfacial adhesion was optimized design. In addition, the aging behavior of plasma treatment on fiber surface was at the primary stage discussed.
In our work, two kinds of organic aramid fibers including Twaron and Armos were modified by oxygen plasma treatment. The fibers reinforced PPESK composite before and after plasma treatment were prepared through solution impregnating process and high temperature molding technique. The changes of fiber surface chemical structure, element composition, surface morphology, surface roughness and surface wettability before and after plasma treatment were characterized by FT-IR spectra, X-ray photoelectron spectroscopy (XPS), scanning electronic microscopy (SEM), atomic force microscopy (AFM) and dynamic contact angle analysis (DCAA) system, respectively. The composite interfacial adhesion property was evaluated by interlaminar shear strength (ILSS), and indirectly illustrated by the water absorption measurements and composite fracture mechanism was analyzed by the morphology of interlaminar shear ruptures of composite observed by SEM.
The effects of oxygen plasma treatment on Twaron aramid fiber surface and its composite interfacial properties were first studied in this paper. The results showed a new oxygen-containing functional group -COO- was introduced onto the fiber surface, the fiber surface roughness increased and the fiber surface wettability was improved obviously after oxygen plasma treatment. Composite interlaminar shear strength increased from 39.2MPa for untreated sample to 52.0MPa for plasma treated for 15min under discharge power at 200 W, with an increase of 32.6%.
Secondly, the influence of plasma treatment condition such as time and discharge power on Armos fiber surface and its composite interfacial properties were studied. It was found that oxygen plasma could introduce a lot of oxygen-containing functional groups onto the fiber surface, the fiber surface was etched obviously and the fiber surface wettability was improved consequently. Composite interlaminar shear strength increased from 59.5MPa for untreated sample to 68.8MPa for plasma treated for 10min under discharge power at 200 W, with an increase of 15.6%. The water absorption of composite decreasing also indirectly showed that oxygen plasma treatment improved composite interfacial adhesion. However, long time and large discharge power would make the fiber surface melting. Then, the fiber surface polar functional group decreased, surface roughness declined and surface wettability degraded. Finally, the composite interfacial properties turned to be weak.
In addition, compared with the morphology of composite interlaminar shear ruptures before and after plasma treatment, it was found that the fibers were smooth with low amount of resin adhered to surface for the untreated specimen, the rupture took place near the interface between the fiber and matrix; However, a large proportion of fibers stuck tightly to matrix, the primary failure mode varied from interface failure to matrix or fiber failure for the oxygen plasma-treated specimen. It suggested that the interfacial bond strengths between the fiber and the matrix were well improved by oxygen plasma treatment. The relationship between the fiber surface characteristics and composite interfacial properties indicated that both the chemical bonding between the fiber and the matrix in composite system and the mechanical interaction contributed for increasing composite interfacial properties.
Finally, the aging behavior of plasma-treated fiber surface was studied. The fiber surface properties such as polar functional groups, surface morphology, surface roughness and surface wettability as a function of storage time in air after plasma treatment were measured. The fiber surface aging behavior could be detected obviously in chemical composition and surface wettability, whereas the surface morphology and roughness remained nearly stable after storing in air as long as 10 days after oxygen plasma treatment. The polar functional groups on fiber surface reorientated or reversaled may be responsible for the weak interfacial strength between the fiber and the matrix in composite system.
引文
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