预浸料生产中智能控制系统的应用

用近红外光谱技术对无碱布/酚醛预浸料的树脂含量、可溶树脂含量和挥发分含量进行在线检测,通过偏最小二乘方法分别建立标准模型,选择光谱预处理方法和PLS的因子数.用近红外方法和标准方法对未知样品进行分析,通过t检验结果显示两种方法没有显著性的差别,利用该方法可以同时预测三项指标,1分钟之内就可以分析一个样品,没有破坏性.如果质量指标不合格,通过自动控制系统发出指令,及时调节工艺参数.研究表明近红外光谱方法能够十分有效和准确对分析预浸料质量.     

The application of near infrared spectroscopy in the quality control analysis of glass/phenolic resin prepreg

During the manufacture of glass/phenolic resin prepreg cloth, the feasibility of near infrared (NIR) spectroscopy as a technique for the quality control analysis of the resin content, the volatile content and the resin pre-curing degree has been verified. The partial least square (PLS) regression was used to develop the calibration models by utilizing several different spectral pretreatments. The optimum models had determination coefficients (R ²) of 98.29 for the resin content, of 99.50 for the volatile content and of 97.66 for the pre-curing degree, respectively. The root mean square errors of prediction (RMSEP) for the resin content, the volatile content and the pre-curing degree were 0.376%, 0.169% and 0.105%, respectively. The results of the paired t-test revealed that there was no significant difference between the NIR method and the standard method. In the manufacture process of the prepreg cloth, the NIR on-line monitoring results were used to be the instructions for the quality control.     

玻璃纤维－环氧树脂预浸料质量控制方法的研究

利用化学分析、红外光谱(IR)、热分析(DSC、TGA)、体积排斥色谱(SEC)等分析技术研究了S2高强玻璃纤维-环氧树脂预浸料在高温(45℃)储存条件下化学特性的变化规律,从而为选择预浸料的质量控制方法提供依据。     

玻璃纤维－环氧树脂预浸料质量控制方法的研究

利用化学分析、红外光谱(IR)、热分析(DSC、TGA)、体积排斥色谱(SEC)等分析技术研究了S2高强玻璃纤维-环氧树脂预浸料在高温(45℃)储存条件下化学特性的变化规律,从而为选择预浸料的质量控制方法提供依据。      

Influence of prepreg conditions on the void occurrence and tensile properties of woven glass fiber-reinforced polyimide composites

The influence of prepreg solvent content on void occurrence in woven glass fiber-reinforced polyimide composites and their tensile properties was studied. A precursor solution of SKYBOND 703 was diluted in an additional solvent (n-methyl pyrrolidone) and the glass woven fabric was immersed in about 40 wt.% polyamic acid, in solvent. Prepregs were dried at 373 K for different time intervals, ranging from 2 to 24 h. Prepregs with varying residual solvent content under each condition were laid up, and their [(0/90)]₄ composite laminates were formed by autoclaving at a hydrostatic pressure of 0.7 MPa. The relationship of drying time with the amount of residual prepreg solvent, as well as with the volume fractions of fiber and voids was investigated. The void geography and content for each composite laminate, and the tensile strength and modulus at room temperature were also evaluated. The results clearly indicated that, depending on the altering residual solvent content in the prepreg, the void geometry and location influenced reduction of the tensile properties of woven fabric composite laminate. An appropriate prepreg resin viscosity during curing, which avoids reduction of the tensile properties, was revealed.     

用近红外光谱技术检测酚醛树脂基高硅氧预浸料质量指标

通过对酚醛树脂基高硅氧预浸料的近红外光谱进行分析,采用化学计量学方法建立了预浸料树脂含量、挥发份含量和预固化度的定量分析模型,研究了光谱预处理方式及光谱区域的选择对定量分析精度的影响。结果表明,用所建立的模型对未知样品预测,树脂含量、挥发份含量和预固化度平均绝对误差分别为0.46%,0.24%和0.42%,可以满足质量检测要求,对生产过程的质量控制具有指导意义。     

连续预浸带的制备工艺研究

本文介绍了用预浸带铺制机湿法制备单向碳纤维预浸带的工艺方法,讨论了影响预浸带树脂含量、外观及挥发分含量的有关因素,优化了工艺条件,确定了制备单向预浸带的最佳工艺参数.制备的预浸带最大宽度为300毫米,连续长度可达200米.可以批量稳定地进行生产.      

Void formation in composite prepregs – Effect of dissolved moisture

Void formation as a function of resin moisture content was investigated to better understand and control process defects in composite parts made from prepreg. In this study, uncured prepreg was conditioned at 70%, 80% and 90% relative humidity and at 35 °C. Conditioned prepreg was laid up into quasi-isotropic laminates and cured using vacuum bag only (VBO) processing (low-pressure), and autoclave processing. Moisture uptake in the resin was measured using coulometric Fischer titration. Void content was measured by image analysis of polished sections of cured laminates. Void fractions increased substantially with increasing moisture content in VBO processed laminates, while autoclave-processed parts remained void-free. Experimental results were consistent with trends predicted using a diffusion-based analytical model. The findings are discussed in the context of causes of voids in prepreg composites.     

玻璃纤维－环氧树脂预浸料的物理化学表征

利用红外光谱等分析测试技术研究了S2高强玻璃纤维-环氧树脂预浸料在不同温度储存条件下,微观结构变化与储存温度之间的关系和在常温储存条件下微观结构与宏观力学性能之间的关系,从而为选择预浸料储存条件提供依据,为预浸料的质量控制提供控制参数和量化指标.      

玻璃纤维－环氧树脂预浸料的物理化学表征

利用红外光谱等分析测试技术研究了S2高强玻璃纤维-环氧树脂预浸料在不同温度储存条件下,微观结构变化与储存温度之间的关系和在常温储存条件下微观结构与宏观力学性能之间的关系,从而为选择预浸料储存条件提供依据,为预浸料的质量控制提供控制参数和量化指标.     

碳纤维增强双马来酰亚胺树脂预浸料铺覆黏性及其储存老化行为

将碳纤维增强双马来酰亚胺树脂预浸料CCM40J/HT-280分别置于4种储存环境（真空、N₂、O₂、空气）进行室温老化实验,研究了预浸料铺覆黏性与储存环境和老化时间的关系,对不同环境下黏性失效前后的样品进行了DSC、流变、红外光谱分析。针对不同黏性级别的预浸料,采用热压罐成型工艺制备了复合材料层合板,对层合板内部成型质量及复合材料力学性能进行了研究。结果表明,真空和N₂环境储存下的CCM40J/HT-280预浸料黏性失效周期相比于O₂与空气中的样品延长约40%。DSC和流变测试结果表明,老化后树脂的交联程度大于新鲜树脂,树脂最低黏度也显著增大,O₂环境下的样品表现的更为明显;对红外光谱特征峰分析表明,O₂环境储存条件下树脂交联反应程度高于真空环境,说明O₂对双马来酰亚胺树脂室温下的老化具有促进作用。黏性失效的预浸料制备的CCM40J/HT-280复合材料内部多为层间或层内的密集孔隙,其弯曲强度下降约13.0%、弯曲模量下降约6.5%,层间剪切强度下降约10.7%。      

牙科复合树脂转化率的测定方法

光聚充填复合树脂是牙齿修复的主要原料之一,在临床使用中,树脂中有机基质分子上碳碳双键的聚合转化率决定着修复的效果和树脂在口腔中的使用寿命。光聚转化率是树脂性能的主要评价指标之一,因此,在研究和使用过程中,树脂光聚转化率的测定十分重要。确定光聚充填复合树脂转化率的方法有多种,目前主要是采用仪器分析的方法。基于傅里叶变换红外光谱(FT-IR)、傅里叶变换拉曼光谱(FT-Raman)、近红外光谱(NIR)、差热分析(DTA)、核磁共振(NMR)和高效液相色谱(HPLC)等仪器在牙科充填复合树脂光聚转化率测定方面的应用,介绍牙科充填复合树脂光聚转化率的测定方法,并分析了各种方法的特点。     

影响蜂窝夹层结构滚筒剥离强度主要因素的研究EI

对预浸料与蜂窝直接接触共固化成形的蜂窝夹层结构的滚筒剥离强度进行了研究，主要讨论了树脂基体、预浸料树脂含量及织物构成对滚筒剥离强度的影响。     

Characterization of a novel natural cellulose fabric from Manicaria saccifera palm as possible reinforcement of composite materials

Identifying novel natural fibers/fabrics with proper properties as reinforcement material is a new challenge in the field of bio-composites. Hence, the aim of this paper is to study the possibility of using a natural fabric extracted from Manicaria saccifera palm as a novel reinforcement in composites. This fabric was extensively characterized by chemical composition analysis, infrared spectroscopy (FTIR) analysis, morphological studies (SEM), thermo-gravimetric analysis (TGA) and physical /mechanical properties studies. From SEM analysis it was identified globular protrusions spread uniformly over the fiber which could help the mechanical interlock with the resin. As well, Manicaria fabric showed good thermal stability, low density, low moisture content and good tensile properties. Further, their properties are comparable to most natural cellulose fabrics and some synthetic fabrics, such as fiber glass fabrics. Manciaria saccifera fabric showed to be a suitable candidate as natural reinforcement material for the development of bio- composite.     

A process model for the compaction and saturation of partially impregnated thermoset prepreg tapes

Automated manufacturing of composite materials is key to reducing cost and improving consistency in part quality. Modeling of manufacturing processes can identify influential material, geometric, and process variables, while providing a framework for their optimization and control. A process model has been formulated to describe the compaction and saturation of partially impregnated thermoset prepreg tapes during their placement, using a roller compaction and vacuum consolidation. The roles of various parameters that characterize the initial prepreg tape state and the final prepreg tape state are investigated. The model yields the degree of resin saturation in the tape with changes in its thickness after being compacted, due to an external pressure. The results estimate the degree of dry fiber region within the tape, which can provide vacuum pathways for air or volatile removal before consolidation and cure. The model can be adapted for different material constitutive relationships of tape compaction and saturation.     

Mechanical properties of aligned multi-walled carbon nanotube/epoxy composites processed using a hot-melt prepreg method

This study examined the mechanical properties of aligned multi-walled carbon nanotube (CNT)/epoxy composites processed using a hot-melt prepreg method. Vertically aligned ultra-long CNT arrays (forest) were synthesized using chemical vapor deposition, and were converted to horizontally aligned CNT sheets by pulling them out. An aligned CNT/epoxy prepreg was fabricated using hot-melting with B-stage cured epoxy resin film. The resin content in prepreg was well controlled. The prepreg sheets showed good drapability and tackiness. Composite film specimens of 24-33 μm thickness were produced, and tensile tests were conducted to evaluate the mechanical properties. The resultant composites exhibit higher Young’s modulus and tensile strength than those of composites produced using conventional CNT/epoxy mixing methods. For example, the maximum elastic modulus and ultimate tensile strength (UTS) of a CNT (21.4 vol.%)/epoxy composite were 50.6 GPa and 183 MPa. These values were, respectively, 19 and 2.9 times those of the epoxy resin.     

Experimental study of damage characteristics of carbon woven fabric/epoxy laminates subjected to lightning strike

This paper experimentally investigates the damage characteristics of two stacking sequenced ([45₂/0₂/−45₂/90₂]s, [30₂/0₂/−30₂/90₂]s) carbon woven fabric/epoxy laminates subjected to simulated lightning strike. Characteristics of the damage are analyzed using visual inspection, image processing, ultrasonic scanning and scanning electron microscope. The mechanical properties of post-lightning specimens are then studied. Observations show that as the lightning strike is intensified, an enlarged resin pyrolized area appears majorly along the weft orientation while the delamination region extends equally to both of the warp and the weft direction. The resin/fiber interfacial bonding is severely damaged by a thermal–mechanical effect due to lightning strike infliction. Mechanical testing further shows that the stacking sequence can influence the failure significantly. Compared with prepreg taped material, the restrained damage area due to special designed stacking sequence, lamina thickness and the weft nylon binder make the woven fabric reinforcement a good choice for the fabrication of lightning protection structures.     

Evaluation of multiblock NIR/MIR PLS predictive models to detect adulteration of diesel/biodiesel blends by vegetal oil

This work investigates the potential of using simultaneously near infrared (NIR) and mid infrared (MIR) spectroscopy for the quantification of vegetable oil in diesel/biodiesel blends. The two spectral ranges were used separately with PLS regressions. To combine the two pieces of information, first a concatenated matrix was used and then H-PLS and S-PLS models were constructed. The models were compared in term of prediction errors (RMSEP). The results obtained in NIR spectroscopy were better than the ones obtained with MIR spectroscopy (considering the influence of the pretreatment and of the selected variables range). The multiblock methodology seems to be of great interest in quantitative analysis with the simultaneous use of information from the MIR and NIR spectroscopy.     

热压罐工艺树脂压力测试系统适用性实验研究

采用玻璃纤维织物/环氧树脂E51预浸料研究热压罐工艺树脂压力在线测试系统适用性,分析了树脂黏度对测试系统动态反应特性的影响,进而测试了热压罐工艺零吸胶条件下等厚、非等厚及L形预浸料铺层内部的树脂压力,并与理论模型计算树脂压力对比,以分析测试系统的准确性。结果表明: 树脂黏度明显影响系统的动态反应特性,当树脂黏度低于25 Pa·s时树脂压力测试系统具有较高的动态反应特性,满足复合材料内部树脂压力测试需求; 对于所研究的各种形式的预浸料铺层,树脂压力测试值与理论值有很好的一致性,当热压罐压力达到0.5 MPa,相对误差约为2%,验证了系统的准确性。     

热压罐零吸胶工艺树脂压力在线测试及其变化规律

针对碳纤维缎纹布/环氧914预浸料热压罐零吸胶工艺,采用热压成型过程树脂压力在线测试系统监测树脂压力的大小与分布,分析了真空、外加气压对树脂压力的作用规律,通过显微观察研究了真空及外加气压对孔隙缺陷的影响。实验结果表明,所采用的在线测试系统可以定量分析真空在铺层内的作用程度和树脂压力的变化;零吸胶工艺树脂承担了大部分外压且沿层板厚度及面内方向分布均匀;真空通过铺层内的气路通道排出夹杂空气,其作用程度受到树脂黏流状态和铺层密实程度的影响;不同压力条件下复合材料层板孔隙状况与树脂压力的测试结果相吻合。