芳纶纤维和芳纶浆粕的结构与芳纶纸特性的相关性研究
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摘要
芳纶纸是由芳纶纤维和芳纶浆粕按一定比例混合抄造而成的特种纤维纸，具有优良的机械性能和耐高温电绝缘性能，广泛用于电气绝缘、航空航天和交通运输等关键领域。高性能芳纶纸是高附加值的电气绝缘纸和结构材料纸，是国家战略性新兴产业重点发展的新材料，其生产技术被美国杜邦公司独家垄断。尽管目前芳纶纸已经国产化，但国产芳纶纸在匀度、强度和色度等方面与杜邦公司的Nomex纸有明显的差距。其主要的原因有两个方面：一是国产芳纶纤维（尤其是芳纶浆粕）本身的性能不是非常适合抄造芳纶纸，另一个原因就是对最优化的芳纶纸微观结构和纤维界面结合状态和机理不太清楚。为了打破高性能芳纶纸生产的技术瓶颈，有必要建立一套有别于传统的植物纤维原料造纸的合成纤维造纸理论，揭示芳纶浆粕纤维结构、热性能、界面结合机理与芳纶纸结构和性能的关系。本研究对芳纶浆粕的结构形态、热性能与芳纶纸结构性能之间的关系进行了深入分析，同时还研究了不同表面改性方法对芳纶纤维表面和芳纶纸结构性能的影响，旨在对适合抄造芳纶纸的芳纶浆粕的结构形态进行分析和表征，对影响芳纶纸强度的主要因素进行评价，阐明芳纶纤维、浆粕在纸张中分布与纸张结构性能的关系，探讨芳纶纤维表面改性方法和芳纶纸界面增强理论，为国内芳纶纤维和芳纶浆粕生产企业提供必要的基础数据和研发目标，为完善纤维表面改性和界面增强技术、优化芳纶纸成形和热压工艺、提高国产芳纶纸质量提供理论及技术支持。
采用鲍尔筛分仪对芳纶浆粕进行筛分，并用纤维分析仪、比表面分析仪、打浆度仪、X-射线衍射仪（XRD）等对各组分浆粕的平均长度、比表面积、打浆度、结晶度、分子质量等形态和结构进行测定，分析了浆粕形态结构与芳纶纸性能的关系。结果表明，芳纶浆粕呈无定形结构，结晶度很低，提高温度及施加外力会提高芳纶浆粕的结晶度。相对分子质量将影响链段活动性从而影响结晶速度，相对分子质量高的要比相对分子质量低的结晶慢。未热压芳纶纸中芳纶短切纤维与芳纶浆粕之间主要是物理混合，浆粕的表面形态对芳纶纸的强度影响较大，芳纶纸强度随着浆粕比表面积和打浆度的增大而增大，与浆粕分子质量和结晶度关系不大。热压后芳纶纸紧度和强度大幅提高，热压后浆粕结晶度越大的，热压芳纶纸紧度越高，空隙率越低，相应的强度越大。中等分子质量的浆粕较适合配抄高强度的热压芳纶纸。
利用示差扫描量热法（DSC）测定了芳纶纤维、不同分子质量芳纶浆粕及不同来源芳纶纸的热性能，分析了芳纶纤维、浆粕及芳纶纸的冷结晶行为、共混组分的相容性和热稳定性。结果表明，芳纶纤维、浆粕及芳纶纸的玻璃化转变温度（Tg）均在270℃以上，三者均具有较好的耐热性能。但三者的Tg存在一定的差异，其中芳纶短切纤维的Tg比芳纶浆粕的略高几度，而芳纶纸的Tg介于两者之间。这主要是由于芳纶短切纤维在生产过程中进行了一定程度的拉伸取向，结晶度较高，从而使其Tg增高，而芳纶浆粕的生产加工方法与芳纶短切纤维不同，其结晶度很低，因此其Tg略低。芳纶纸是由芳纶短切纤维与芳纶浆粕以一定比例混合抄制而成的，所以其Tg介于短切纤维与浆粕之间。芳纶纸只出现了一个玻璃化转变温度，这说明芳纶浆粕和芳纶短切纤维在一定程度上是相容的。
芳纶短切纤维、芳纶浆粕和自制芳纶纸在高于Tg时均会产生冷结晶现象，其中芳纶浆粕的冷结晶温度远高于芳纶短切纤维，而冷结晶放热量低于芳纶短切纤维，说明芳纶浆粕通过冷结晶来提高结晶完善程度的潜力较大一些。芳纶短切纤维、芳纶浆粕和自制芳纶纸的熔融温度（Tm）在430~445℃之间，短切纤维的Tm最高，熔融吸热量最大，芳纶浆粕最小。由于芳纶纸由芳纶浆粕和短切纤维以一定比例混合抄造而成，分子质量分布较宽，吸热反应较缓慢，因此其熔程最长。芳纶浆粕和自制芳纶纸在480~495℃会出现明显的热裂解峰。
芳纶浆粕的玻璃化转变温度Tg、Tm和热裂解温度(Td)均随着分子质量的增大而提高，其耐热性能与其分子质量及分子质量分布的均匀性密切相关。各种不同分子质量的芳纶浆粕均在385~395℃之间出现冷结晶峰。
两种国产纸的Tm和熔融吸热量都高于杜邦公司的Nomex纸，即国产芳纶纸的耐热性能优于Nomex纸，但Nomex纸的吸热峰宽△T小于两种国产芳纶纸，说明其分子质量的均一性优于国产芳纶纸，这可能是其物理强度性能优于国产芳纶纸的原因之一。
利用动态热机械分析仪（DMA）研究自制芳纶纸、杜邦公司的Nomex纸与纯浆粕芳纶纸热压前后的储能模量、损耗模量和损耗因子等参数随温度变化的关系，结合结晶度的变化，研究不同芳纶纸的玻璃化转变、链段松弛等结构差异和变化过程，分析芳纶纤维原料结构、热压工艺对芳纶纸机械性能的影响。结果表明，自制芳纶纸热压前后的Tg均比Nomex纸略高，这说明自制芳纶纸的耐热性能较好，这与所用芳纶纤维和浆粕的分子质量较高有关。但热压前自制芳纶纸的储能模量远远低于Nomex411纸，这一方面与芳纶本身的结晶度相关，另一方面与芳纶纸中短切纤维和浆粕的界面粘合情况有关，较低的初始结晶度和较差的芳纶纤维/浆粕界面粘合是导致自制未热压芳纶纸的储能模量和强度远低于Nomex411纸的根本原因。热压使得自制芳纶纸、Nomex410纸和纯浆粕芳纶纸的模量大幅提高。升温使得芳纶浆粕部分熔融，在压力作用下比表面积增大，与芳纶纤维结合力增强，同时在热压过程中芳纶分子链重排，变得更规整，分子链取向度和结晶度提高，分子间相互作用力增大，从而提高了芳纶纸的模量和物理强度。由于自制未热压芳纶纸中芳纶纤维分布杂乱而无规律，所以在热压后成纸中仍存在一些空隙，芳纶纤维与浆粕的结合不及Nomex410纸紧密，导致自制热压芳纶纸的模量和强度不及Nomex410纸。
利用各种纸张匀度表征方法分析了芳纶纸匀度、纤维的定向分布等结构特性对纸张性能的影响。结果表明，β射线匀度仪和微扫描匀度仪的匀度表征方法与热压前芳纶纸的物理强度有较好的相关性，未热压芳纶纸的定量标准偏差越大，其抗张强度和撕裂度越小，微扫描法测定出来的匀度指数越高，则未热压芳纶纸的物理强度越大。热压后芳纶纸的抗张强度与定量标准偏差和Paper Perfect Formation (PPF)匀度值的相关性较好，但撕裂度与各种匀度测定结果没有明确的相关性。
纸张表面小尺寸的云彩花较多对芳纶纸的强度是不利的，而大尺寸云彩花的存在对芳纶纸的强度是有利的。改变芳纶纸的抄造工艺，使更多的浆粕存在于纸张表面，则热压后纸张表面平滑度、质感将会更好，其强度也将更大。
热压后芳纶纸的抗张挺度取向（TSO）远大于普通的书写、印刷及包装类纸张。两种国产芳纶纸和自制芳纶纸的纵横向抗张挺度指数及抗张挺度指数纵横向比均低于Nomex410纸。国产芳纶纸的模量低是其抗张挺度低的主要原因，而抗张挺度纵横向比低是与成形工艺、热压工艺相关的。改变抄纸工艺和热压工艺，尽可能地改善纤维的取向，同时避免热压时对芳纶纸的过分压紧，对提高芳纶纸纵向抗张挺度指数和抗张挺度指数纵横向比是有益的。
在相同定量下，自制热压芳纶纸的透气度高于Nomex410纸，而两种国产机制芳纶纸的透气度更高，其紧度反而比Nomex410纸大。采用分层抄造技术，在芳纶纸表面覆盖更多的薄膜状浆粕，有利于提高芳纶纸表面的致密性，降低其透气度，对于改善芳纶纸的强度性能及电气性能是有益的，同时还可提高芳纶纸的平滑度。
热压过程中芳纶浆粕表面化学结构发生了变化，从而导致芳纶纸白度下降，在芳纶纸中添加含铋的氧化物可抑制热压过程中纸面发生氧化，减轻纸张的返黄，但纸张的抗张强度没有明显变化。
对芳纶纤维进行不同浓度的磷酸改性、硅烷偶联剂改性、硝化/还原改性和NaOH改性，然后以改性后的芳纶纤维配抄芳纶纸。结果表明，20%的磷酸溶液处理芳纶纤维后，使其表面粗化，纤维表面含氧量提高，改善了芳纶纤维与浆粕间的结合，从而提高了芳纶纸的抗张强度和撕裂度。硅烷偶联剂改性、硝化还原法改性、NaOH改性均不同程度地改善了芳纶纤维与浆粕的结合能力，提高了芳纶纸的物理强度。相比而言，20%的磷酸溶液改性对提高芳纶纸强度效果最好，偶联剂法和NaOH改性法次之，而硝化还原改性对提高芳纶纸的抗张性能和撕裂性能效果较差。
Aramid papers are specialty papers made from aramid fibers and aramidpulp, which are well known for their excellent mechanical properties, hightemperature resistance and electrical insulating property, and are widely used inelectrical insulation, aviation, transportation and other key areas. Highperformance aramid paper is a high value-added electrical insulating paper andstructural material paper, is the strategic new material of our country, but theproduction technology of it is exclusively monopolized by the Dupont Company.Though aramid papers are achieved domestically currently, domestic aramidpapers are obviously weaker in formation, strength and color than Nomex papers.The reasons mainly lie in two aspects: firstly, demestic aramid fiber (especiallyaramid pulp) itself is not quite suitable for making aramid paper; secondly, theoptimum aramid paper microscopic structure and fiber interface bonding stateand mechanism are not very clear, which limits the production technologicalimprovement of high performance aramid paper. To break the technicalbottleneck of high performance aramid paper production, it is necessary toestablish a set of new synthetic fiber papermaking theory which is different fromthe traditional papermaking theory, to reveal the relationship between fiberstructure, thermal properties, interfacial bonding and paper structure, paperproperties. In this research, the relationship between the structure and thermalproperties of aramid pulp and the structure and properties of aramid papers hasbeen analyzed, and the influence of different surface modification methods onthe fiber surface structure and aramid paper structure has also been investigated.The aim is to analyze and characterize the optimum configuration of aramidpulp for making aramid papers, to evaluate the main factors influencing thestrength of aramid paper, to elaborate the relationship between the distribution of aramid fibers and aramid pulp and the structure and properties of aramid paper;to discuss fiber surface modification mechanism and its effect on the interfacialbonding properties, thereby provide necessary basic data and development goalsfor domestic aramid fiber production enterprises, and provide theoretical andtechnical support for improving fiber surface modification and interfaceenhancement technology, as well as for optimizing the forming and hotcalendaring technology of aramid papers to improve their quality.
Bauer screen was used to screen the aramid pulp, and fiber quality analyzer,BET specific surface area analyzer, Schopper-Riegler beating degree tester,X-Ray Diffraction (XRD) and other methods were used to determine the averagefiber length, specific surface area, beating degree, crystallinity, and molecularweight of aramid pulp, and the relationship between the structure of aramid pulpand the properties of aramid papers was discussed. Results show aramid pulp isamorphous, and has lower crystallinity. Increasing the temperature and exertingpressure can improve the crystallinity of aramid pulp, and the molecular weightof aramid pulp has an effect on the crystallization rate. The crystallization rate ofaramid pulp with higher molecular weight is lower than that of aramid pulp withlower molecular weight. Aramid fibers and aramid pulp in uncalendered aramidpapers are bonded by simple physical blend, so the surface morphology ofaramid pulp is the fundamental determinant of the uncalendered aramid paperstrength, and the strength of uncalendered aramid papers improves with theincrease of specific surface area and beating degree of aramid pulp, however, themolecular weight and crystallinity of aramid pulp have little influence on theuncalendered aramid paper strength. After hot calendaring, the density andstrength of aramid papers are greatly increased, and the higher the crystallinityand density, the lower the porosity, the higher the paper strength. Aramid pulpwith medium molecular weight is suitable for making high strength aramidpaper.
Differential Scanning Calorimetry (DSC) was used to determine the thermalperformance parameters of aramid fibers, aramid pulp with different molecularweight and aramid papers of different sources, and cold crystallization behavior,component compatibility and thermostability of aramid fibers, aramid pulp andaramid papers were analyzed. Results show that the glass transition temperature (Tg) of aramid fibers, aramid pulp and aramid papers are all higher than270℃,that is, they all have good heat resistance. However, they are different from eachother, and among them, the Tgof aramid fibers is higher that that of aramid pulp,and the Tgof aramid papers is in between. This is because that aramid fibers havehigh crystallinity after stretch orientation in the process of production, butaramid pulp has different process from aramid fibers, and it has low crystallinity.Aramid papers are made from the mixture of aramid fibers and aramid pulp, soits Tgis in between aramid fibers and aramid pulp. Furthermore, aramid papershave only one Tg, which indicates that the two components in aramid papershave good compatibility.
Cold crystallization peak was also observed in the DSC of aramid fibers,aramid pulp and aramid papers when the temperature is higher than the Tg, andcompared with aramid fibers, aramid pulp has higher cold crystallizationtemperature and lower cold crystal enthalpy, and it indicates that aramid pulp hasgreater potential in increasing crystallinity through cold crystallization. Themelting temperature of aramid fibers, aramid pulp and aramid papers are in therange of430~445℃, and aramid fibers has the highest melting temperature andheat absorption capacity, but aramid pulp has the lowest melting temperature andheat absorption capacity. Because aramid paper is made from aramid fibers andaramid pulp, and it has wider molecular weight distribution, so its endothermicreaction is the slowest and its melting range is the longest. For aramid pulp andself-made aramid paper, there appears obvious pyrolysis peak when thetemperature is in the range of480~495℃.
The glass transition temperature Tg, melting temperature and pyrolysistemperature of aramid pulp increase with the increase of its molecular weight,which indicates that the heat resistance of aramid pulp is closely related to itsmolecular weight and the uniformity of its molecular weight distribution. Thereare cold crystallization peaks in the temperature range of385~395℃for aramidpulp with different molecular weight.
The melting temperature and heat absorption capacity of two domesticaramid papers (MetaStarTMand X-Fiper) are higher than that of Nomex papers,that is, the heat resistance of domestic aramid papers are superior to that ofNomex papers. However, Nomex papers have narrower endothermic peak than the two domestic aramid papers, which indicates that Nomex papers have moreuniform molecular weight distribution, and this may be one of the reasons fortheir superior physical strength.
Dynamic Mechanical Analyzer (DMA) was used to discuss the storagemodulus, loss modulus and loss factor of self-made aramid papers, Nomexpapers and pure aramid pulp paper before and after hot pressing, and to find howthese parameters change with temperature. Combined with the changes incrystallinity, the glass transition, relaxation of the chain segments and otherstructure differences and change process of different aramid papers werediscussed, thereby analyzing the influence of fiber structure and hot pressing onthe physical properties of aramid papers. The results show that the Tgofself-made aramid before and after hot pressing are a little higher than that ofNomex papers, self-made aramid papers have better heat resistance, and thisresults from the higher molecular weight of aramid fibers and aramid pulps.However, the storage modulus of self-made aramid papers before hot pressingare far less than that of Nomex411papers. On the one hand, it is related to thecrystallinity of aramid raw materials, on the other hand, it is related to theinterfacial bonding between aramid fibers and aramid pulp. The lower initialcrystallinity and weaker interfacial bonding make the modulus and strength ofself-made uncalendered aramid papers far lower than that of Nomex papers. Hotpressing significantly improves the modulus of self-made aramid papers, Nomex410papers and pure pulp aramid papers. Heating makes aramid pulp partlymolten, and the specific surface area of aramid pulp increases under the pressure,which increases the interfacial bonding between aramid pulp and fibers.Meanwhile, aramid molecular chains rearrange and become more regular duringhot pressing, which improves the orientation and crystallinity of molecularchains, and increases the molecular interaction, thus improving the modulus andphysical strength of aramid papers. Because fiber distribution in self-madeuncalendered aramid papers is disorderly and irregualarly, after hot pressing,there are still some voids in self-made aramid papers, and the interfacial bondingbetween aramid fibers and pulp in self-made aramid papers is less than that inNomex410papers, which leading to a lower modulus and strength of self-madearamid papers than that of Nomex410papers.
Various kinds of characterization methods were used to analyze the effectsof paper formation, fiber orientation distribution on paper properties. Resultsshow that β Formation Tester and Micro-scanner Formation Analyzer aresuitable for uncalendered aramid papers, and the paper formation characterizedby these two methods have good relation with the physical strength of aramidpapers. The bigger the basis weight standard deviation of uncalendered aramidsheets, the less the tensile strength and tear strength of them, and the higher theformation index by Micro-scanner formation analyzer, the higher physicalstrength of uncalendered aramid papers. After hot pressing, the tensile strengthof aramid papers have good relations with their basis weight standard deviationand Paper Perfect Formation (PPF) values, but there is no clear correlationbetween the tear strength of aramid papers and their formation determinationresults.
Small size clouds on the surface of aramid papers is unfavorable to thestrength of aramid papers, while large size clouds on paper surface is beneficialto the strength of aramid papers. Changing papermaking technology andallowing more aramid pulp deposit onto the surface of paper will improve thesurface smoothness and texture of aramid papers, thus improves their physicalstrength.
Tensile stiffness orientation angle (TSOAngle) of calendered aramid papers isfar larger than that of the common writing paper, printing paper and packagingpaper. The tensile stiffness index in machine direction (TSIMD), tensile stiffnessindex in cross machine direction (TSICD) and TSIMD/CDof two domestic aramidpapers and self-made aramid papers are all lower than that of Nomex410papers.The lower tensile stiffness of domestic aramid papers mainly due to their lowermodulus, and the lower TSIMD/CDof domestic aramid papers relates to theirforming and hot-pressing technology. Changing the papermaking technology andhot-pressing technology to improve the fiber orientation as far as possible andavoiding overcompaction during hot pressing are useful for improving the TSIMDand TSIMD/CDof aramid papers.
Air permeability of self-made aramid papers, especially air permeability oftwo domestic aramid papers are higher than that of Nomex410papers with thesame basis weight, but the density of Nomex410papers are lower than that of self-made and two domestic aramid papers. Multi-ply forming can let morearamid pulp cover on the surface of aramid paper like a thin film, therebyimproves the surface density of aramid paper and decreases its air permeability,which is beneficial to improve the smoothness, strength property and electricalperformance of aramid papers.
Hot pressing decreases the whiteness of aramid papers, and surfacefunctional groups change of aramid pulp during hot pressing is perhaps the majorreason. Addition of bismuth oxide or bismuth nitrate into aramid paper caninhibit oxidation and reduce whiteness reversion of aramid paper during hotpressing, however, the tensile strength of aramid paper has no obviously change.
In this work, surface modification of aramid fibers were performed by usingdifferent consistency of phosphoric acid solution (PA), silane coupling agent(KH-550), nitration/reduction agent and sodium hydroxide solution (NaOH),respectively, and modified aramid fibers were used to make aramid papers witharamid pulp, then the optimal modifying process was studied. Results show thattreatment with20%phosphoric acid solution roughs the surface of aramid fibersand increases the oxygen content of fiber surface, thus improves the interfacialbonding between aramid fibers and aramid pulp and increases the tensile strengthand tear strength of aramid papers. Surface modification of aramid fibers bysilane coupling agent, nitration/reduction agents and NaOH can all increase thebonding between aramid fibers and aramid pulp at a certain extent, and improvethe tensile strength and tear strength of aramid papers. In contrast, surfacemodification with20%phosphoric acid has the best effect on improving thestrength of aramid papers, silane coupling agent and NaOH modification areworse than20%phosphoric acid, but better than nitration/reductionmodification.
采用鲍尔筛分仪对芳纶浆粕进行筛分，并用纤维分析仪、比表面分析仪、打浆度仪、X-射线衍射仪（XRD）等对各组分浆粕的平均长度、比表面积、打浆度、结晶度、分子质量等形态和结构进行测定，分析了浆粕形态结构与芳纶纸性能的关系。结果表明，芳纶浆粕呈无定形结构，结晶度很低，提高温度及施加外力会提高芳纶浆粕的结晶度。相对分子质量将影响链段活动性从而影响结晶速度，相对分子质量高的要比相对分子质量低的结晶慢。未热压芳纶纸中芳纶短切纤维与芳纶浆粕之间主要是物理混合，浆粕的表面形态对芳纶纸的强度影响较大，芳纶纸强度随着浆粕比表面积和打浆度的增大而增大，与浆粕分子质量和结晶度关系不大。热压后芳纶纸紧度和强度大幅提高，热压后浆粕结晶度越大的，热压芳纶纸紧度越高，空隙率越低，相应的强度越大。中等分子质量的浆粕较适合配抄高强度的热压芳纶纸。
利用示差扫描量热法（DSC）测定了芳纶纤维、不同分子质量芳纶浆粕及不同来源芳纶纸的热性能，分析了芳纶纤维、浆粕及芳纶纸的冷结晶行为、共混组分的相容性和热稳定性。结果表明，芳纶纤维、浆粕及芳纶纸的玻璃化转变温度（Tg）均在270℃以上，三者均具有较好的耐热性能。但三者的Tg存在一定的差异，其中芳纶短切纤维的Tg比芳纶浆粕的略高几度，而芳纶纸的Tg介于两者之间。这主要是由于芳纶短切纤维在生产过程中进行了一定程度的拉伸取向，结晶度较高，从而使其Tg增高，而芳纶浆粕的生产加工方法与芳纶短切纤维不同，其结晶度很低，因此其Tg略低。芳纶纸是由芳纶短切纤维与芳纶浆粕以一定比例混合抄制而成的，所以其Tg介于短切纤维与浆粕之间。芳纶纸只出现了一个玻璃化转变温度，这说明芳纶浆粕和芳纶短切纤维在一定程度上是相容的。
芳纶短切纤维、芳纶浆粕和自制芳纶纸在高于Tg时均会产生冷结晶现象，其中芳纶浆粕的冷结晶温度远高于芳纶短切纤维，而冷结晶放热量低于芳纶短切纤维，说明芳纶浆粕通过冷结晶来提高结晶完善程度的潜力较大一些。芳纶短切纤维、芳纶浆粕和自制芳纶纸的熔融温度（Tm）在430~445℃之间，短切纤维的Tm最高，熔融吸热量最大，芳纶浆粕最小。由于芳纶纸由芳纶浆粕和短切纤维以一定比例混合抄造而成，分子质量分布较宽，吸热反应较缓慢，因此其熔程最长。芳纶浆粕和自制芳纶纸在480~495℃会出现明显的热裂解峰。
芳纶浆粕的玻璃化转变温度Tg、Tm和热裂解温度(Td)均随着分子质量的增大而提高，其耐热性能与其分子质量及分子质量分布的均匀性密切相关。各种不同分子质量的芳纶浆粕均在385~395℃之间出现冷结晶峰。
两种国产纸的Tm和熔融吸热量都高于杜邦公司的Nomex纸，即国产芳纶纸的耐热性能优于Nomex纸，但Nomex纸的吸热峰宽△T小于两种国产芳纶纸，说明其分子质量的均一性优于国产芳纶纸，这可能是其物理强度性能优于国产芳纶纸的原因之一。
利用动态热机械分析仪（DMA）研究自制芳纶纸、杜邦公司的Nomex纸与纯浆粕芳纶纸热压前后的储能模量、损耗模量和损耗因子等参数随温度变化的关系，结合结晶度的变化，研究不同芳纶纸的玻璃化转变、链段松弛等结构差异和变化过程，分析芳纶纤维原料结构、热压工艺对芳纶纸机械性能的影响。结果表明，自制芳纶纸热压前后的Tg均比Nomex纸略高，这说明自制芳纶纸的耐热性能较好，这与所用芳纶纤维和浆粕的分子质量较高有关。但热压前自制芳纶纸的储能模量远远低于Nomex411纸，这一方面与芳纶本身的结晶度相关，另一方面与芳纶纸中短切纤维和浆粕的界面粘合情况有关，较低的初始结晶度和较差的芳纶纤维/浆粕界面粘合是导致自制未热压芳纶纸的储能模量和强度远低于Nomex411纸的根本原因。热压使得自制芳纶纸、Nomex410纸和纯浆粕芳纶纸的模量大幅提高。升温使得芳纶浆粕部分熔融，在压力作用下比表面积增大，与芳纶纤维结合力增强，同时在热压过程中芳纶分子链重排，变得更规整，分子链取向度和结晶度提高，分子间相互作用力增大，从而提高了芳纶纸的模量和物理强度。由于自制未热压芳纶纸中芳纶纤维分布杂乱而无规律，所以在热压后成纸中仍存在一些空隙，芳纶纤维与浆粕的结合不及Nomex410纸紧密，导致自制热压芳纶纸的模量和强度不及Nomex410纸。
利用各种纸张匀度表征方法分析了芳纶纸匀度、纤维的定向分布等结构特性对纸张性能的影响。结果表明，β射线匀度仪和微扫描匀度仪的匀度表征方法与热压前芳纶纸的物理强度有较好的相关性，未热压芳纶纸的定量标准偏差越大，其抗张强度和撕裂度越小，微扫描法测定出来的匀度指数越高，则未热压芳纶纸的物理强度越大。热压后芳纶纸的抗张强度与定量标准偏差和Paper Perfect Formation (PPF)匀度值的相关性较好，但撕裂度与各种匀度测定结果没有明确的相关性。
纸张表面小尺寸的云彩花较多对芳纶纸的强度是不利的，而大尺寸云彩花的存在对芳纶纸的强度是有利的。改变芳纶纸的抄造工艺，使更多的浆粕存在于纸张表面，则热压后纸张表面平滑度、质感将会更好，其强度也将更大。
热压后芳纶纸的抗张挺度取向（TSO）远大于普通的书写、印刷及包装类纸张。两种国产芳纶纸和自制芳纶纸的纵横向抗张挺度指数及抗张挺度指数纵横向比均低于Nomex410纸。国产芳纶纸的模量低是其抗张挺度低的主要原因，而抗张挺度纵横向比低是与成形工艺、热压工艺相关的。改变抄纸工艺和热压工艺，尽可能地改善纤维的取向，同时避免热压时对芳纶纸的过分压紧，对提高芳纶纸纵向抗张挺度指数和抗张挺度指数纵横向比是有益的。
在相同定量下，自制热压芳纶纸的透气度高于Nomex410纸，而两种国产机制芳纶纸的透气度更高，其紧度反而比Nomex410纸大。采用分层抄造技术，在芳纶纸表面覆盖更多的薄膜状浆粕，有利于提高芳纶纸表面的致密性，降低其透气度，对于改善芳纶纸的强度性能及电气性能是有益的，同时还可提高芳纶纸的平滑度。
热压过程中芳纶浆粕表面化学结构发生了变化，从而导致芳纶纸白度下降，在芳纶纸中添加含铋的氧化物可抑制热压过程中纸面发生氧化，减轻纸张的返黄，但纸张的抗张强度没有明显变化。
对芳纶纤维进行不同浓度的磷酸改性、硅烷偶联剂改性、硝化/还原改性和NaOH改性，然后以改性后的芳纶纤维配抄芳纶纸。结果表明，20%的磷酸溶液处理芳纶纤维后，使其表面粗化，纤维表面含氧量提高，改善了芳纶纤维与浆粕间的结合，从而提高了芳纶纸的抗张强度和撕裂度。硅烷偶联剂改性、硝化还原法改性、NaOH改性均不同程度地改善了芳纶纤维与浆粕的结合能力，提高了芳纶纸的物理强度。相比而言，20%的磷酸溶液改性对提高芳纶纸强度效果最好，偶联剂法和NaOH改性法次之，而硝化还原改性对提高芳纶纸的抗张性能和撕裂性能效果较差。
Aramid papers are specialty papers made from aramid fibers and aramidpulp, which are well known for their excellent mechanical properties, hightemperature resistance and electrical insulating property, and are widely used inelectrical insulation, aviation, transportation and other key areas. Highperformance aramid paper is a high value-added electrical insulating paper andstructural material paper, is the strategic new material of our country, but theproduction technology of it is exclusively monopolized by the Dupont Company.Though aramid papers are achieved domestically currently, domestic aramidpapers are obviously weaker in formation, strength and color than Nomex papers.The reasons mainly lie in two aspects: firstly, demestic aramid fiber (especiallyaramid pulp) itself is not quite suitable for making aramid paper; secondly, theoptimum aramid paper microscopic structure and fiber interface bonding stateand mechanism are not very clear, which limits the production technologicalimprovement of high performance aramid paper. To break the technicalbottleneck of high performance aramid paper production, it is necessary toestablish a set of new synthetic fiber papermaking theory which is different fromthe traditional papermaking theory, to reveal the relationship between fiberstructure, thermal properties, interfacial bonding and paper structure, paperproperties. In this research, the relationship between the structure and thermalproperties of aramid pulp and the structure and properties of aramid papers hasbeen analyzed, and the influence of different surface modification methods onthe fiber surface structure and aramid paper structure has also been investigated.The aim is to analyze and characterize the optimum configuration of aramidpulp for making aramid papers, to evaluate the main factors influencing thestrength of aramid paper, to elaborate the relationship between the distribution of aramid fibers and aramid pulp and the structure and properties of aramid paper;to discuss fiber surface modification mechanism and its effect on the interfacialbonding properties, thereby provide necessary basic data and development goalsfor domestic aramid fiber production enterprises, and provide theoretical andtechnical support for improving fiber surface modification and interfaceenhancement technology, as well as for optimizing the forming and hotcalendaring technology of aramid papers to improve their quality.
Bauer screen was used to screen the aramid pulp, and fiber quality analyzer,BET specific surface area analyzer, Schopper-Riegler beating degree tester,X-Ray Diffraction (XRD) and other methods were used to determine the averagefiber length, specific surface area, beating degree, crystallinity, and molecularweight of aramid pulp, and the relationship between the structure of aramid pulpand the properties of aramid papers was discussed. Results show aramid pulp isamorphous, and has lower crystallinity. Increasing the temperature and exertingpressure can improve the crystallinity of aramid pulp, and the molecular weightof aramid pulp has an effect on the crystallization rate. The crystallization rate ofaramid pulp with higher molecular weight is lower than that of aramid pulp withlower molecular weight. Aramid fibers and aramid pulp in uncalendered aramidpapers are bonded by simple physical blend, so the surface morphology ofaramid pulp is the fundamental determinant of the uncalendered aramid paperstrength, and the strength of uncalendered aramid papers improves with theincrease of specific surface area and beating degree of aramid pulp, however, themolecular weight and crystallinity of aramid pulp have little influence on theuncalendered aramid paper strength. After hot calendaring, the density andstrength of aramid papers are greatly increased, and the higher the crystallinityand density, the lower the porosity, the higher the paper strength. Aramid pulpwith medium molecular weight is suitable for making high strength aramidpaper.
Differential Scanning Calorimetry (DSC) was used to determine the thermalperformance parameters of aramid fibers, aramid pulp with different molecularweight and aramid papers of different sources, and cold crystallization behavior,component compatibility and thermostability of aramid fibers, aramid pulp andaramid papers were analyzed. Results show that the glass transition temperature (Tg) of aramid fibers, aramid pulp and aramid papers are all higher than270℃,that is, they all have good heat resistance. However, they are different from eachother, and among them, the Tgof aramid fibers is higher that that of aramid pulp,and the Tgof aramid papers is in between. This is because that aramid fibers havehigh crystallinity after stretch orientation in the process of production, butaramid pulp has different process from aramid fibers, and it has low crystallinity.Aramid papers are made from the mixture of aramid fibers and aramid pulp, soits Tgis in between aramid fibers and aramid pulp. Furthermore, aramid papershave only one Tg, which indicates that the two components in aramid papershave good compatibility.
Cold crystallization peak was also observed in the DSC of aramid fibers,aramid pulp and aramid papers when the temperature is higher than the Tg, andcompared with aramid fibers, aramid pulp has higher cold crystallizationtemperature and lower cold crystal enthalpy, and it indicates that aramid pulp hasgreater potential in increasing crystallinity through cold crystallization. Themelting temperature of aramid fibers, aramid pulp and aramid papers are in therange of430~445℃, and aramid fibers has the highest melting temperature andheat absorption capacity, but aramid pulp has the lowest melting temperature andheat absorption capacity. Because aramid paper is made from aramid fibers andaramid pulp, and it has wider molecular weight distribution, so its endothermicreaction is the slowest and its melting range is the longest. For aramid pulp andself-made aramid paper, there appears obvious pyrolysis peak when thetemperature is in the range of480~495℃.
The glass transition temperature Tg, melting temperature and pyrolysistemperature of aramid pulp increase with the increase of its molecular weight,which indicates that the heat resistance of aramid pulp is closely related to itsmolecular weight and the uniformity of its molecular weight distribution. Thereare cold crystallization peaks in the temperature range of385~395℃for aramidpulp with different molecular weight.
The melting temperature and heat absorption capacity of two domesticaramid papers (MetaStarTMand X-Fiper) are higher than that of Nomex papers,that is, the heat resistance of domestic aramid papers are superior to that ofNomex papers. However, Nomex papers have narrower endothermic peak than the two domestic aramid papers, which indicates that Nomex papers have moreuniform molecular weight distribution, and this may be one of the reasons fortheir superior physical strength.
Dynamic Mechanical Analyzer (DMA) was used to discuss the storagemodulus, loss modulus and loss factor of self-made aramid papers, Nomexpapers and pure aramid pulp paper before and after hot pressing, and to find howthese parameters change with temperature. Combined with the changes incrystallinity, the glass transition, relaxation of the chain segments and otherstructure differences and change process of different aramid papers werediscussed, thereby analyzing the influence of fiber structure and hot pressing onthe physical properties of aramid papers. The results show that the Tgofself-made aramid before and after hot pressing are a little higher than that ofNomex papers, self-made aramid papers have better heat resistance, and thisresults from the higher molecular weight of aramid fibers and aramid pulps.However, the storage modulus of self-made aramid papers before hot pressingare far less than that of Nomex411papers. On the one hand, it is related to thecrystallinity of aramid raw materials, on the other hand, it is related to theinterfacial bonding between aramid fibers and aramid pulp. The lower initialcrystallinity and weaker interfacial bonding make the modulus and strength ofself-made uncalendered aramid papers far lower than that of Nomex papers. Hotpressing significantly improves the modulus of self-made aramid papers, Nomex410papers and pure pulp aramid papers. Heating makes aramid pulp partlymolten, and the specific surface area of aramid pulp increases under the pressure,which increases the interfacial bonding between aramid pulp and fibers.Meanwhile, aramid molecular chains rearrange and become more regular duringhot pressing, which improves the orientation and crystallinity of molecularchains, and increases the molecular interaction, thus improving the modulus andphysical strength of aramid papers. Because fiber distribution in self-madeuncalendered aramid papers is disorderly and irregualarly, after hot pressing,there are still some voids in self-made aramid papers, and the interfacial bondingbetween aramid fibers and pulp in self-made aramid papers is less than that inNomex410papers, which leading to a lower modulus and strength of self-madearamid papers than that of Nomex410papers.
Various kinds of characterization methods were used to analyze the effectsof paper formation, fiber orientation distribution on paper properties. Resultsshow that β Formation Tester and Micro-scanner Formation Analyzer aresuitable for uncalendered aramid papers, and the paper formation characterizedby these two methods have good relation with the physical strength of aramidpapers. The bigger the basis weight standard deviation of uncalendered aramidsheets, the less the tensile strength and tear strength of them, and the higher theformation index by Micro-scanner formation analyzer, the higher physicalstrength of uncalendered aramid papers. After hot pressing, the tensile strengthof aramid papers have good relations with their basis weight standard deviationand Paper Perfect Formation (PPF) values, but there is no clear correlationbetween the tear strength of aramid papers and their formation determinationresults.
Small size clouds on the surface of aramid papers is unfavorable to thestrength of aramid papers, while large size clouds on paper surface is beneficialto the strength of aramid papers. Changing papermaking technology andallowing more aramid pulp deposit onto the surface of paper will improve thesurface smoothness and texture of aramid papers, thus improves their physicalstrength.
Tensile stiffness orientation angle (TSOAngle) of calendered aramid papers isfar larger than that of the common writing paper, printing paper and packagingpaper. The tensile stiffness index in machine direction (TSIMD), tensile stiffnessindex in cross machine direction (TSICD) and TSIMD/CDof two domestic aramidpapers and self-made aramid papers are all lower than that of Nomex410papers.The lower tensile stiffness of domestic aramid papers mainly due to their lowermodulus, and the lower TSIMD/CDof domestic aramid papers relates to theirforming and hot-pressing technology. Changing the papermaking technology andhot-pressing technology to improve the fiber orientation as far as possible andavoiding overcompaction during hot pressing are useful for improving the TSIMDand TSIMD/CDof aramid papers.
Air permeability of self-made aramid papers, especially air permeability oftwo domestic aramid papers are higher than that of Nomex410papers with thesame basis weight, but the density of Nomex410papers are lower than that of self-made and two domestic aramid papers. Multi-ply forming can let morearamid pulp cover on the surface of aramid paper like a thin film, therebyimproves the surface density of aramid paper and decreases its air permeability,which is beneficial to improve the smoothness, strength property and electricalperformance of aramid papers.
Hot pressing decreases the whiteness of aramid papers, and surfacefunctional groups change of aramid pulp during hot pressing is perhaps the majorreason. Addition of bismuth oxide or bismuth nitrate into aramid paper caninhibit oxidation and reduce whiteness reversion of aramid paper during hotpressing, however, the tensile strength of aramid paper has no obviously change.
In this work, surface modification of aramid fibers were performed by usingdifferent consistency of phosphoric acid solution (PA), silane coupling agent(KH-550), nitration/reduction agent and sodium hydroxide solution (NaOH),respectively, and modified aramid fibers were used to make aramid papers witharamid pulp, then the optimal modifying process was studied. Results show thattreatment with20%phosphoric acid solution roughs the surface of aramid fibersand increases the oxygen content of fiber surface, thus improves the interfacialbonding between aramid fibers and aramid pulp and increases the tensile strengthand tear strength of aramid papers. Surface modification of aramid fibers bysilane coupling agent, nitration/reduction agents and NaOH can all increase thebonding between aramid fibers and aramid pulp at a certain extent, and improvethe tensile strength and tear strength of aramid papers. In contrast, surfacemodification with20%phosphoric acid has the best effect on improving thestrength of aramid papers, silane coupling agent and NaOH modification areworse than20%phosphoric acid, but better than nitration/reductionmodification.
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