可变长纤维增强反应注射成型技术及其制品质量控制研究
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摘要
可变长纤维增强反应注射成型(Variable Long Fiber Reinforced Reaction Injection Molding, VLFRRIM)技术是在增强反应注射成型和可变纤维注入技术基础上发展而来的新型复合材料成型技术,虽然在一定的领域得到应用,但VLFRRIM技术基础理论研究则较为匮乏和滞后。本文以减少VLFRRIM制品缺陷,提高质量为目标,采用理论分析与试验相结合的方法,探索VLFRRIM工艺条件、材料形态结构演化与制品性能之间的影响规律,以实现对VLFRRIM制品提高质量、降低成本的目标,最后利用研究得到的较优工艺参数制备了汽车内饰件产品,验证了本研究方案的可行性。主要研究内容如下：
(1)综合一般反应注射成型理论,研究了工艺原理、材料体系、设备系统、制品及模具结构设计等VLFRRIM关键技术,归纳了制品常见缺陷并对其产生原因进行了分析,为汽车内饰件等同类制品的开发提供了一整套完整的VLFRRIM技术解决方案。
(2)研究了纤维种类(玻璃纤维、植物纤维和碳纤维及其混杂纤维)、纤维含量和长度、模具温度、混合料温、合模压力等主要工艺参数对长纤维渗透率的影响,构建了工艺参数与渗透率关系模型,结果表明各工艺参数均对渗透率有较显著的影响；采用绝热温升实验建立了基料聚合时的反应动力学模型,该模型可以有效预测聚合时体系的温度、异氰酸酯转化率,以及充模和固化过程中模腔内的温度变化；采用动态DSC方法研究了VLFRRIM混合物料体系的固化动力学行为,重点研究了不同纤维的加入对聚氨酯体系的固化动力学方程、反应活化能、反应级数的影响,结果表明纤维加入后,混合物料表观活化能和指前因子显著增加,最大增加到原来的2倍,在相同升温速率下的最大固化反应速率降低,固化持续时间延长,反应级数均为1左右；运用流动指数和密度分布系数对VLFRRIM混合物料体系的流动性进行了表征,研究了纤维种类、纤维含量和长度、模具温度和混合料温等工艺参数对流动性的影响,当纤维长度达到25mm以上,质量百分含量大于30%时,混合物料的流动性显著降低。
(3)研究了纤维种类、纤维含量和长度、模具温度、混合料温、纤维表面处理方式、在模时间、后熟化温度和时间等诸多成型工艺参数对VLFRRIM制品拉伸性能、弯曲性能和冲击性能等力学性能以及热下垂等尺寸稳定性能的影响,结果表明各类长纤维的加入均可提高VLFRRIM制品的力学性能与尺寸稳定性,纤维含量和长度对VLFRRIM制品性能的影响较显著,同时探讨了VLFRRIM复合材料形态结构演化与力学性能的关系。采用热失重法对聚氨酯及其复合材料进行了热失重分析,结果表明VLFRRIM复合材料在200℃时会发生少量分解,表明其具有较好的热稳定性。通过实验方法考察了纤维种类、纤维含量和长度、模具温度、混合料温、后熟化温度和时间等工艺参数对VLFRRIM制品复原性、翘曲变形量等表观质量的影响,其中纤维含量和长度的增加可以显著改善制品的表观质量。
(4)基于纤维复合材料应力传递理论和层合板理论,在相关研究基础上,综合考虑了纤维性能的分散性,纤维的长度分布、取向分布和强度分布,以及泡孔结构、大小及面密度对复合材料性能的影响,构建了适合于VLFRRIM复合材料的模量预测模型、拉伸强度和冲击强度预测模型,研究结果表明,当纤维质量百分含量小于15%,表明预测值与实验值符合度较好,纤维百分含量大于15%时,预测误差较大。
(5)以纤维含量、纤维长度、模具温度、混合料温、在模时间、物料配比等作为工艺参数,采用Taguchi方法进行正交试验设计,分析各种工艺参数对VLFRRIM制品综合性能的影响,得到了多个指标的优化工艺参数；运用模糊加权综合评价法对VLFRRIM制品弯曲模量、冲击强度和翘曲变形量进行总体优化,获得了较佳优化工艺参数组合。与某企业结合,利用本文研究成果试制了某型号挖掘机下挂,结果该制品的各项性能指标均有较大提高,废品率明显下降,同时减少了基料用量,节约了成本。
Variable long fiber reinforced reaction injection molding (VLFRRIM) is a new process for composite material molding technology which was developed based on reinforced reaction injection molding and variable fiber injection technology.Although to be applied in some of the areas, the basic theory research of VLFRRIM technology is deficient and lag. In order to reduce VLFRRIM products'defect, improve VLFRRIM products'quality, in this paper, the mutual influence discipline of VLFRRIM important processing conditions、 evolution of Material forms structuren the morphology and properties of VLFRRIM products have been systemically investigated through the theoretical analysis and test. The results of these studies have therefore achieve the goal of VLFRRIM products'quality improving and cost of production reducing, finally, The preparation of car inner decoration products according to the best optimal process parameters from this study, verify the feasibility of our research project. The main research contents are as follows:
(1) Research on the VLFRRIM key technology such as process theory, material system, equipment system, VLFRRIM products and mould structure design systemically through the theoretical of reinforced reaction injection molding. Sum up the VLFRRIM products'common defects and analyzes its reasons,then, developed a whole solution project for the development of VLFRRIM products of Car inner decoration.
(2) Effects of the main processing parameters such as type of fiber (glass fiber, plant fiber, carbon fiber), fiber contents and length, mold material temperature, mixture material temperature and compound die pressure on the permeability of long fiber were discussed, established a model which respect to technology parameters and permeability. It proves that each technology parameters have significant effect on permeability; The reaction kinetics mode during makings polymerization was established through adiabatic temperature rise experiments and brookfield rheometer, this model can exactly predict the curves of the temperature of the Makings system, the conversion of isocyanate and the mold cavity temperature during filling and curing; Research on curing kinetics of VLFRRIM mixture material system with dynamic DSC test, focus on the influence of dynamic equation, reaction activation energy, reaction series during inject different fiber into PU system. It turn out that,with injection of fiber, the apparent activation energy and the former factor have a significant increase(The best fiber injection can increase2times to the original), In the same heating rate, reduces the max curing reaction rate, extends curing reaction time, whatmore, each reaction order is about1;Fluidity of VLFRRIM mixture material system get characterization with flow index and density distribution coefficient, Effects of processing parameters such as type of fiber, fiber contents and length, mold material temperature on the fluidity were discussed. The study revealed that when length of fiber up to25mm, fiber contents exceed30%, fluidity of mixture material have a significant reduce.
(3) Effects of various processing parameters such as type of fiber, contents and length of fiber, time of compound die, temperature and time of later aging on mechanical property such as tensile property, bending property and impact property, and hot prolapsed dimensional stability of VLFRRIM products were researched,the study revealed that injection of every type of fiber can improve mechanical property and dimensional stability of VLFRRIM products, among various processing parameters, contents and length of fiber are significant factors to property of VLFRRIM products, moreover, the relation between morphological structure evolution of VLFRRIM material and mechanical property is taked into research. Mass loss of VLFRRIM material get analysis through thermogravimetry, the result indicates that VLFRRIM material, which start disintegrate at the temperature of200℃has a good heat stability. Effects of processing parameters such as type of fiber, fiber contents and length, mold material temperature, mixture material temperature and compound die pressure on surface quality of VLFRRIM products such as restoration and warpage amount were discussed, with the increasing of fiber contents and length, surface quality of VLFRRIM products get a significantly improve.
(4) Based on stress transmission theory of fiber composites and laminated plate theory, effects of dispersion of fiber properties, length distribution, orientation distribution and intensity distribution of fiber, as well as foam pore structure, size, and surface density on the property of the composite were synthetically considered, established prediction models of modulus, tensile strength and impact strength which respect to VLFRRIM material. The results show that when the fiber weight percent is less than15%, the equations were better in agreement with the experimental results, but when the fiber weight percent is more than15%, the prediction error is relatively large.
(5) Designed orthogonal test with Taguchi method, effects of the main processing parameters such as fiber contents, fiber length, mold material temperature, mixture material temperature and time of compound die, the mass ratio of material on combination property of VLFRRIM products were analysised, Got the optimization of process parameters of several index; Conceptual optimized the bending modulus, impact strength and warping deformation through comprehensive valuation equation, obtain the optimum set of processing parameters. Combining with enterprise, prepared inner decoration products of car with the optimum set of processing parameters and other research techniques in this article, results shows that the products of VLFRRIM have better combination property, while reducing the amount of base material, and cost savings.
(1)综合一般反应注射成型理论,研究了工艺原理、材料体系、设备系统、制品及模具结构设计等VLFRRIM关键技术,归纳了制品常见缺陷并对其产生原因进行了分析,为汽车内饰件等同类制品的开发提供了一整套完整的VLFRRIM技术解决方案。
(2)研究了纤维种类(玻璃纤维、植物纤维和碳纤维及其混杂纤维)、纤维含量和长度、模具温度、混合料温、合模压力等主要工艺参数对长纤维渗透率的影响,构建了工艺参数与渗透率关系模型,结果表明各工艺参数均对渗透率有较显著的影响；采用绝热温升实验建立了基料聚合时的反应动力学模型,该模型可以有效预测聚合时体系的温度、异氰酸酯转化率,以及充模和固化过程中模腔内的温度变化；采用动态DSC方法研究了VLFRRIM混合物料体系的固化动力学行为,重点研究了不同纤维的加入对聚氨酯体系的固化动力学方程、反应活化能、反应级数的影响,结果表明纤维加入后,混合物料表观活化能和指前因子显著增加,最大增加到原来的2倍,在相同升温速率下的最大固化反应速率降低,固化持续时间延长,反应级数均为1左右；运用流动指数和密度分布系数对VLFRRIM混合物料体系的流动性进行了表征,研究了纤维种类、纤维含量和长度、模具温度和混合料温等工艺参数对流动性的影响,当纤维长度达到25mm以上,质量百分含量大于30%时,混合物料的流动性显著降低。
(3)研究了纤维种类、纤维含量和长度、模具温度、混合料温、纤维表面处理方式、在模时间、后熟化温度和时间等诸多成型工艺参数对VLFRRIM制品拉伸性能、弯曲性能和冲击性能等力学性能以及热下垂等尺寸稳定性能的影响,结果表明各类长纤维的加入均可提高VLFRRIM制品的力学性能与尺寸稳定性,纤维含量和长度对VLFRRIM制品性能的影响较显著,同时探讨了VLFRRIM复合材料形态结构演化与力学性能的关系。采用热失重法对聚氨酯及其复合材料进行了热失重分析,结果表明VLFRRIM复合材料在200℃时会发生少量分解,表明其具有较好的热稳定性。通过实验方法考察了纤维种类、纤维含量和长度、模具温度、混合料温、后熟化温度和时间等工艺参数对VLFRRIM制品复原性、翘曲变形量等表观质量的影响,其中纤维含量和长度的增加可以显著改善制品的表观质量。
(4)基于纤维复合材料应力传递理论和层合板理论,在相关研究基础上,综合考虑了纤维性能的分散性,纤维的长度分布、取向分布和强度分布,以及泡孔结构、大小及面密度对复合材料性能的影响,构建了适合于VLFRRIM复合材料的模量预测模型、拉伸强度和冲击强度预测模型,研究结果表明,当纤维质量百分含量小于15%,表明预测值与实验值符合度较好,纤维百分含量大于15%时,预测误差较大。
(5)以纤维含量、纤维长度、模具温度、混合料温、在模时间、物料配比等作为工艺参数,采用Taguchi方法进行正交试验设计,分析各种工艺参数对VLFRRIM制品综合性能的影响,得到了多个指标的优化工艺参数；运用模糊加权综合评价法对VLFRRIM制品弯曲模量、冲击强度和翘曲变形量进行总体优化,获得了较佳优化工艺参数组合。与某企业结合,利用本文研究成果试制了某型号挖掘机下挂,结果该制品的各项性能指标均有较大提高,废品率明显下降,同时减少了基料用量,节约了成本。
Variable long fiber reinforced reaction injection molding (VLFRRIM) is a new process for composite material molding technology which was developed based on reinforced reaction injection molding and variable fiber injection technology.Although to be applied in some of the areas, the basic theory research of VLFRRIM technology is deficient and lag. In order to reduce VLFRRIM products'defect, improve VLFRRIM products'quality, in this paper, the mutual influence discipline of VLFRRIM important processing conditions、 evolution of Material forms structuren the morphology and properties of VLFRRIM products have been systemically investigated through the theoretical analysis and test. The results of these studies have therefore achieve the goal of VLFRRIM products'quality improving and cost of production reducing, finally, The preparation of car inner decoration products according to the best optimal process parameters from this study, verify the feasibility of our research project. The main research contents are as follows:
(1) Research on the VLFRRIM key technology such as process theory, material system, equipment system, VLFRRIM products and mould structure design systemically through the theoretical of reinforced reaction injection molding. Sum up the VLFRRIM products'common defects and analyzes its reasons,then, developed a whole solution project for the development of VLFRRIM products of Car inner decoration.
(2) Effects of the main processing parameters such as type of fiber (glass fiber, plant fiber, carbon fiber), fiber contents and length, mold material temperature, mixture material temperature and compound die pressure on the permeability of long fiber were discussed, established a model which respect to technology parameters and permeability. It proves that each technology parameters have significant effect on permeability; The reaction kinetics mode during makings polymerization was established through adiabatic temperature rise experiments and brookfield rheometer, this model can exactly predict the curves of the temperature of the Makings system, the conversion of isocyanate and the mold cavity temperature during filling and curing; Research on curing kinetics of VLFRRIM mixture material system with dynamic DSC test, focus on the influence of dynamic equation, reaction activation energy, reaction series during inject different fiber into PU system. It turn out that,with injection of fiber, the apparent activation energy and the former factor have a significant increase(The best fiber injection can increase2times to the original), In the same heating rate, reduces the max curing reaction rate, extends curing reaction time, whatmore, each reaction order is about1;Fluidity of VLFRRIM mixture material system get characterization with flow index and density distribution coefficient, Effects of processing parameters such as type of fiber, fiber contents and length, mold material temperature on the fluidity were discussed. The study revealed that when length of fiber up to25mm, fiber contents exceed30%, fluidity of mixture material have a significant reduce.
(3) Effects of various processing parameters such as type of fiber, contents and length of fiber, time of compound die, temperature and time of later aging on mechanical property such as tensile property, bending property and impact property, and hot prolapsed dimensional stability of VLFRRIM products were researched,the study revealed that injection of every type of fiber can improve mechanical property and dimensional stability of VLFRRIM products, among various processing parameters, contents and length of fiber are significant factors to property of VLFRRIM products, moreover, the relation between morphological structure evolution of VLFRRIM material and mechanical property is taked into research. Mass loss of VLFRRIM material get analysis through thermogravimetry, the result indicates that VLFRRIM material, which start disintegrate at the temperature of200℃has a good heat stability. Effects of processing parameters such as type of fiber, fiber contents and length, mold material temperature, mixture material temperature and compound die pressure on surface quality of VLFRRIM products such as restoration and warpage amount were discussed, with the increasing of fiber contents and length, surface quality of VLFRRIM products get a significantly improve.
(4) Based on stress transmission theory of fiber composites and laminated plate theory, effects of dispersion of fiber properties, length distribution, orientation distribution and intensity distribution of fiber, as well as foam pore structure, size, and surface density on the property of the composite were synthetically considered, established prediction models of modulus, tensile strength and impact strength which respect to VLFRRIM material. The results show that when the fiber weight percent is less than15%, the equations were better in agreement with the experimental results, but when the fiber weight percent is more than15%, the prediction error is relatively large.
(5) Designed orthogonal test with Taguchi method, effects of the main processing parameters such as fiber contents, fiber length, mold material temperature, mixture material temperature and time of compound die, the mass ratio of material on combination property of VLFRRIM products were analysised, Got the optimization of process parameters of several index; Conceptual optimized the bending modulus, impact strength and warping deformation through comprehensive valuation equation, obtain the optimum set of processing parameters. Combining with enterprise, prepared inner decoration products of car with the optimum set of processing parameters and other research techniques in this article, results shows that the products of VLFRRIM have better combination property, while reducing the amount of base material, and cost savings.
引文
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