无卤阻燃GF/PA66的界面相容性与性能研究
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摘要
玻纤增强尼龙广泛应用于电子、电气、汽车等领域，因此无卤阻燃玻纤增强尼龙新材料的研究和开发是十分重要的，特别是于2006年7月1日正式实施欧盟RoHS指令，《关于在电子电气设备中限制使用某些有害物质指令》，对无卤阻燃材料的研究更得到了各国的高度重视，产品的市场需求也更加迫切。
对玻纤增强材料，其最终性能不仅取决于增强体和基质的性质，而且也决定于两相界面的性质。作为基质和增强体间的桥梁，界面是复合材料非常重要的微观结构，其对材料的物理、化学和机械性能都有着重要的影响，然而纤维和基质尼龙间的作用是较弱的，因此改善的界面粘结程度是非常重要的，也是复合材料研究的热点。
为了解决玻纤增强尼龙的界面及阻燃性能，本文采用无卤阻燃剂聚磷酸蜜胺盐MPP来制备高性能无卤阻燃玻璃纤维增强尼龙66，用FTIR，XRD，DSC，DMA和SEM等手段对材料的界面和性能进行表征。结果表明，在MPP添加量为25％，玻璃纤维25％，界面改性剂MA-EPDM 7％，各种助剂为1％时，玻纤增强尼龙66可达到UL941.6mm V-0级，并具有良好的力学性能：拉伸强度大于140MPa，弯曲强度大于210MPa，冲击强度8.5kJ·m-~(2)，确定了适于该体系的双螺杆组合参数，加工工艺参数，注塑工艺等条件。
采用DSC法对尼龙66复合材料等温结晶和熔融行为进行研究，用Avrami方程对动力学过程进行分析。研究发现阻燃剂MPP的加入对尼龙66的结晶行为产生了很大影响，MPP对尼龙66有着较强的异相成核作用，使得复合材料中尼龙66结晶速率加快；但是MPP的存在，提高了界面间相互作用，同时又阻碍了尼龙66分子链的自由运动，使得球晶尺寸变小，结晶度并未显著增加；对等温结晶样品的熔融行为研究发现，所有的样品呈熔融双峰，这主要是由于尼龙66不同尺寸和完善程度的结晶以及升温过程中的再结晶和再熔融引起的，阻燃剂对尼龙66的晶态结构影响较小，XRD中的结晶峰位并未发生明显变化。
采用DSC法对尼龙66复合材料非等温结晶行为进行研究，用Avrami、Kissinger和Ozawa模型对非等温结晶动力学进行处理。结果表明，该方法能够比较好地处理尼龙66及其复合材料的非等温结晶动力学。非等温结晶过程中，玻纤也起到了成核作用，使结晶速度大幅度增加；MPP对尼龙66的异相成核的作用，同时由于界面粘结的改善，也阻碍了尼龙66分子链运动，使得复合材料的结晶速率并未大幅度提高，这与等温结晶的结果有一定的偏差，说明非等温结晶过程更为复杂。采用XRD，DSC及POM相结合的方法研究了阻燃剂对尼龙66晶态结构的影响，结果显示尼龙66及其复合材料中都出现了多重结晶现象。
力学性能研究表明，阻燃剂在提高材料阻燃性能的同时，使复合材料拉伸强度、弯曲强度、储能模量、玻璃化转变温度、松弛活化能都得到提高，说明体系界面粘结强度的提高，这进一步证实了界面粘结情况的改善。
采用热重分析(TGA)研究了复合材料的热稳定性，结果表明，阻燃剂的存在，降低了尼龙66的热稳定性，提高了成炭能力，改善了阻燃性能。
流变性能研究表明，尼龙66表现为牛顿流体，而在复合材料中表现为假塑性流体。通过活化能研究确定了适于阻燃玻纤增强尼龙66体系的加工温度为275℃，阻燃剂的加入，增加了体系的粘度和粘流活化能，也说明了材料界面相互作用的增强。
总之，MPP的加入，增加了玻纤与尼龙基质间的界面粘结，提高了材料的阻燃及力学性能。
Glass fiber (GF) reinforced nylon has been widely used in many fields such as electric, electronic, automobile, etc, so the study and expoitation of non-halogen flame retardant glass fiber reinforced nylon new materials is very important. Especially RollS enforcement was delivered on the 1 st July 2006. The RollS Directive stands for "the restriction of the use of certain hazardous substances in electrical and electronic equipment". It makes many countries take remarkable consideration of the non-halogen materials and the demands of product's market are more imminence.
The whole properties of composites relate to not only reinforcement phase and matrix phase, but also the interface between these two phases. Interface is a very important micro- structure of composites. As the bridge between reinforcement fiber and matrix, the interface has an important effect on the physical, chemical and mechanical properties of composites. However, the interface between fiber and matrix is the weak area in composites which are reinforced by fiber, therefore the improvement of interfacial adhesion, as the hotspot in composite research, is of great significance.
In this paper, aiming at solving the problem of interface and flame retardancy, on the base of our previous work, we prepared the flame retardant through the reaction of melamine and polyphosphoric acid. FTIR, XRD, DSC, DMA and SEM were used to characterize the interface and properties. Upon the addition of 25%MPP, 25%GF, 7%MA-EPDM, 1% additives, the flame retarded GF reinforced PA66 reached UL 94 V-O rating at 1.6mm thickness, and possessed good mechanical properties, tensile strength more than 140MPa, flexural strength more than 210 MPa and impact strength 8.5 kJ.m~(-2). We also got the screw configuration, processing parameters, injection parameters, etc.
The effect of MPP on the isothermal crystallization and melting behavior of PA66 was investigated by differential scanning calorimetry (DSC). The Avrami equation was used to describe the isothermal crystallization kinetics. It is indicated that the MPP act as effective heterogeneous nucleating agents, the crystallization rate of PA 66 in the composites is thus increased. However the MPP inhinders the motion of PA66 chains, thus reduce the crystal spherulite radius of PA66. The flame retarded composites exhibit double melting endotherms during researched crystallization temperature. The multiple melting endotherms are mainly caused by the recrystallization of PA66 spherulites with different crystal sizes and imperfection during heating. The MPP have little effect on the crystalline structure of PA66 under isothermal condition, which can be proved by XRD.
The non-isothermal crystallization and melting behavior of PA66 and its composites were investigated by DSC. The Avrami, Kissinger, Ozawa equations are used to describe the non- isothermal crystallization kinetics. The results show that those equations can all describe the nonisothermal crystallization process. The addition of MPP into PA66 has an effect on the mechanism of nucleation and the growth of PA66 crystallites. The MPP and glass fiber all act as nucleating agents, but MPP hinders the motion of PA66 chains which resulted in the decrease of crystallization rate. The result is different from the isothermal process, indicating the complexity of non-isothermal crystallization. A combination of DSC, XRD and polarized microscopy (POM) was used to investigate the effect of MPP on the crystallization structure of PA66, the results showed the phenomena of multi-crystalline.
The mechaniacal properties of PA66 composites were investigated. It is found that MPP cause the tensile strength, flexural strength, storage modulus, glass transiton temperature (Tg) and relaxation activation energy to increase. The better properties of the composites result from the stronger interfacial adhesion between GF and PA66.
The thermal degradation behavior of GF/PA66/MPP composites was studied using thermogravimetric analysis (TGA). The presence of MPP decreased the thermal stability of PA66, which showed that MPP accelerated the formation of char of nylon 66 reinforced with glass fiber and enhanced the flame retardancy.
From the rheology properties study, PA66 exhibited Newtonian fluid behavior, and the composites exhibited the shear thinning behavior. The introduction of MPP increased the viscosity and flow activation energy of GF/PA66 composites. The research of activation energy showed that the processing temperature fitted in the industrial production is at 275℃for GF/PA66/MPP. The stronger rheological effect of MPP results from stronger matrix-fillers interactions.
In all, MPP improves the compatibility between the GF and PA66, resulting in stronger interfacial adhesion.
对玻纤增强材料，其最终性能不仅取决于增强体和基质的性质，而且也决定于两相界面的性质。作为基质和增强体间的桥梁，界面是复合材料非常重要的微观结构，其对材料的物理、化学和机械性能都有着重要的影响，然而纤维和基质尼龙间的作用是较弱的，因此改善的界面粘结程度是非常重要的，也是复合材料研究的热点。
为了解决玻纤增强尼龙的界面及阻燃性能，本文采用无卤阻燃剂聚磷酸蜜胺盐MPP来制备高性能无卤阻燃玻璃纤维增强尼龙66，用FTIR，XRD，DSC，DMA和SEM等手段对材料的界面和性能进行表征。结果表明，在MPP添加量为25％，玻璃纤维25％，界面改性剂MA-EPDM 7％，各种助剂为1％时，玻纤增强尼龙66可达到UL941.6mm V-0级，并具有良好的力学性能：拉伸强度大于140MPa，弯曲强度大于210MPa，冲击强度8.5kJ·m-~(2)，确定了适于该体系的双螺杆组合参数，加工工艺参数，注塑工艺等条件。
采用DSC法对尼龙66复合材料等温结晶和熔融行为进行研究，用Avrami方程对动力学过程进行分析。研究发现阻燃剂MPP的加入对尼龙66的结晶行为产生了很大影响，MPP对尼龙66有着较强的异相成核作用，使得复合材料中尼龙66结晶速率加快；但是MPP的存在，提高了界面间相互作用，同时又阻碍了尼龙66分子链的自由运动，使得球晶尺寸变小，结晶度并未显著增加；对等温结晶样品的熔融行为研究发现，所有的样品呈熔融双峰，这主要是由于尼龙66不同尺寸和完善程度的结晶以及升温过程中的再结晶和再熔融引起的，阻燃剂对尼龙66的晶态结构影响较小，XRD中的结晶峰位并未发生明显变化。
采用DSC法对尼龙66复合材料非等温结晶行为进行研究，用Avrami、Kissinger和Ozawa模型对非等温结晶动力学进行处理。结果表明，该方法能够比较好地处理尼龙66及其复合材料的非等温结晶动力学。非等温结晶过程中，玻纤也起到了成核作用，使结晶速度大幅度增加；MPP对尼龙66的异相成核的作用，同时由于界面粘结的改善，也阻碍了尼龙66分子链运动，使得复合材料的结晶速率并未大幅度提高，这与等温结晶的结果有一定的偏差，说明非等温结晶过程更为复杂。采用XRD，DSC及POM相结合的方法研究了阻燃剂对尼龙66晶态结构的影响，结果显示尼龙66及其复合材料中都出现了多重结晶现象。
力学性能研究表明，阻燃剂在提高材料阻燃性能的同时，使复合材料拉伸强度、弯曲强度、储能模量、玻璃化转变温度、松弛活化能都得到提高，说明体系界面粘结强度的提高，这进一步证实了界面粘结情况的改善。
采用热重分析(TGA)研究了复合材料的热稳定性，结果表明，阻燃剂的存在，降低了尼龙66的热稳定性，提高了成炭能力，改善了阻燃性能。
流变性能研究表明，尼龙66表现为牛顿流体，而在复合材料中表现为假塑性流体。通过活化能研究确定了适于阻燃玻纤增强尼龙66体系的加工温度为275℃，阻燃剂的加入，增加了体系的粘度和粘流活化能，也说明了材料界面相互作用的增强。
总之，MPP的加入，增加了玻纤与尼龙基质间的界面粘结，提高了材料的阻燃及力学性能。
Glass fiber (GF) reinforced nylon has been widely used in many fields such as electric, electronic, automobile, etc, so the study and expoitation of non-halogen flame retardant glass fiber reinforced nylon new materials is very important. Especially RollS enforcement was delivered on the 1 st July 2006. The RollS Directive stands for "the restriction of the use of certain hazardous substances in electrical and electronic equipment". It makes many countries take remarkable consideration of the non-halogen materials and the demands of product's market are more imminence.
The whole properties of composites relate to not only reinforcement phase and matrix phase, but also the interface between these two phases. Interface is a very important micro- structure of composites. As the bridge between reinforcement fiber and matrix, the interface has an important effect on the physical, chemical and mechanical properties of composites. However, the interface between fiber and matrix is the weak area in composites which are reinforced by fiber, therefore the improvement of interfacial adhesion, as the hotspot in composite research, is of great significance.
In this paper, aiming at solving the problem of interface and flame retardancy, on the base of our previous work, we prepared the flame retardant through the reaction of melamine and polyphosphoric acid. FTIR, XRD, DSC, DMA and SEM were used to characterize the interface and properties. Upon the addition of 25%MPP, 25%GF, 7%MA-EPDM, 1% additives, the flame retarded GF reinforced PA66 reached UL 94 V-O rating at 1.6mm thickness, and possessed good mechanical properties, tensile strength more than 140MPa, flexural strength more than 210 MPa and impact strength 8.5 kJ.m~(-2). We also got the screw configuration, processing parameters, injection parameters, etc.
The effect of MPP on the isothermal crystallization and melting behavior of PA66 was investigated by differential scanning calorimetry (DSC). The Avrami equation was used to describe the isothermal crystallization kinetics. It is indicated that the MPP act as effective heterogeneous nucleating agents, the crystallization rate of PA 66 in the composites is thus increased. However the MPP inhinders the motion of PA66 chains, thus reduce the crystal spherulite radius of PA66. The flame retarded composites exhibit double melting endotherms during researched crystallization temperature. The multiple melting endotherms are mainly caused by the recrystallization of PA66 spherulites with different crystal sizes and imperfection during heating. The MPP have little effect on the crystalline structure of PA66 under isothermal condition, which can be proved by XRD.
The non-isothermal crystallization and melting behavior of PA66 and its composites were investigated by DSC. The Avrami, Kissinger, Ozawa equations are used to describe the non- isothermal crystallization kinetics. The results show that those equations can all describe the nonisothermal crystallization process. The addition of MPP into PA66 has an effect on the mechanism of nucleation and the growth of PA66 crystallites. The MPP and glass fiber all act as nucleating agents, but MPP hinders the motion of PA66 chains which resulted in the decrease of crystallization rate. The result is different from the isothermal process, indicating the complexity of non-isothermal crystallization. A combination of DSC, XRD and polarized microscopy (POM) was used to investigate the effect of MPP on the crystallization structure of PA66, the results showed the phenomena of multi-crystalline.
The mechaniacal properties of PA66 composites were investigated. It is found that MPP cause the tensile strength, flexural strength, storage modulus, glass transiton temperature (Tg) and relaxation activation energy to increase. The better properties of the composites result from the stronger interfacial adhesion between GF and PA66.
The thermal degradation behavior of GF/PA66/MPP composites was studied using thermogravimetric analysis (TGA). The presence of MPP decreased the thermal stability of PA66, which showed that MPP accelerated the formation of char of nylon 66 reinforced with glass fiber and enhanced the flame retardancy.
From the rheology properties study, PA66 exhibited Newtonian fluid behavior, and the composites exhibited the shear thinning behavior. The introduction of MPP increased the viscosity and flow activation energy of GF/PA66 composites. The research of activation energy showed that the processing temperature fitted in the industrial production is at 275℃for GF/PA66/MPP. The stronger rheological effect of MPP results from stronger matrix-fillers interactions.
In all, MPP improves the compatibility between the GF and PA66, resulting in stronger interfacial adhesion.
引文
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