Stress and Strain During the Process of Thermal Stabilization of Modified Pan Precursors

Thermal mechanical analysis, FT- IR, WAXD and some conventional measurements, such as densities and mechanical properties, were used to characterize the effect of the modification using KMnO4 and SnCl4 on the thermal mechanical behaviors and structural changes dining the process of thermal stabilization of modified PAN precursors. to the unmodified original PAN precursors, some conclusions were drawn that the thermal stabilization starts at a lower temperature for modified PAN fibers, for example, the peak of thermal stress changes for modified PAN precursors using KMnO4 displays a decrease of 20℃ and a increase of 30% in the ultimate thermal stress, that chemical modification makes structural transformation perfect and increases by 25% of the thermal stress at the temperature range of 230℃- 300℃, that the modified PAN fibers display an increase of 100% in the thermal strain, once after pre-oxidized, show an increase of 7.8% in orientation index, and a decrease of 9.9% in crystal size for identical preload in the region of 13.1 - 14.5 MPa. It was also concluded that the modification using SnCl4 would alleviate the changes in physical and chemical stress regimes and result in improvement in structure and decrease in defects.     

聚丙烯腈改性碳纳米管复合材料的电性能

采用溶液聚合的方法制备聚丙烯腈,对聚丙烯腈进行热处理改性后,与碳纳米管共混制备复合材料.与未改性处理的复合材料相比,电导率提高了2个多数量级.用FTIR、Raman和XPS等方法进行研究,结果表明聚丙烯腈经热处理改性后,部分腈基(—C=N)转变为亚胺基(-C=N),其链状结构向环状结构转化,MWNTs上的π电子与改性后聚丙烯腈的π电子之间形成强的π-π共轭,增强了改性聚丙烯腈与碳纳米管之间的相互作用,提高了复合材料的导电性能.     

力场效应在聚丙烯腈分子热分解环化初期的作用

采用X-射线衍射、声速仪和红外光谱研究了聚丙烯腈(PAN)纤维在分子热分解—环化演变初期张力的作用,结果表明：在PAN纤维氰基热分解环化初期,张力可以增加纤维中分子聚集态结构的有序化程度;有利于PAN纤维构型的转变和完善原丝原有结构,随张力的增大,PAN纤维的全取向度和结晶度也是增加的;另外,张力可以促进PAN纤维分子的热分解环化反应,尤其是分子内的环化反应,当牵伸达到4%以后可以使微晶尺寸变小,这对提高纤维强度是有利的。     

Si/C复合纳米纤维负极材料的制备及其性能表征

以聚丙烯晴（PAN）作为高分子聚合物配体和碳源, 并添加少量纳米硅粉, 利用静电纺丝方法制备Si/C复合负极材料. 用热重分析（TG）研究前驱体的分解过程, 用X射线衍射（XRD）、 Raman光谱和扫描电子显微镜（SEM）研究Si/C复合材料的晶体结构和微观形貌. 结果表明: Si/C复合材料具有纳米纤维结构, 纤维直径约
为350 nm, 呈交错的网状分布; PAN高温分解产物多为无定形碳; 材料在0.1,0.2,0.5,1.0,2.0 C下的放电容量分别为735.6,712.1,685.4,492.3,367.9 mA·h/g, 其倍率性能较好.     

静电纺丝制备复合纳米纤维聚丙烯腈/纳米纤维素晶体/银及其性能

采用静电纺丝技术, 以N,N-二甲基甲酰胺为溶剂, 聚丙烯腈为载体, 制备复合纳米纤维聚丙烯腈/纳米纤维素晶体/银, 并用Fourier变换红外光谱（FT-IR）、 透射电子显微镜（TEM）、 扫描电子显微镜（SEM）、 差热 热重分析（TG-DTG）和X射线衍射（XRD）等方法对复合纳米纤维的化学结构、 形貌、 热稳定性和晶体结构进行表征. 结果表明： 聚丙烯腈、 纳米纤维素晶体和银纳米粒子有机结合形成复合纳米纤维聚丙烯腈/纳米纤维素晶体/银; 复合纳米纤维的尺寸均匀, 平均直径为（214±12）nm, Ag纳米粒子在复合纳米纤维体系中均匀分布, 粒径为5~25 nm; 该复合纳米纤维对金黄色葡萄球菌和大肠杆菌的抗菌性能优异.     

MnO2/C复合纳米纤维纱线的制备及其导电性能

采用共轭静电纺丝法制备聚丙烯腈(PAN)纳米纤维纱线,并在不同温度下将PAN纳米纤维碳化得到碳纳米纤维纱线。以KMnO 4为锰源,通过水热合成法在碳纳米纤维纱线上原位生长纳米二氧化锰(MnO 2),形成MnO 2/C复合纳米纤维纱线,分别采用傅里叶变换红外光谱(FTIR)、扫描电子显微镜(SEM)、场发射扫描电子显微镜(FE-SEM)、数字万用表对碳纳米纤维纱线和MnO 2/C复合纳米纤维纱线的化学组成、表观形貌、电学性能等进行表征,并分析碳化温度对碳纳米纤维纱线的形貌和电学性能的影响,以及水热反应中盐酸浓度对纳米MnO 2形貌和MnO 2/C复合纳米纤维纱线的影响。结果表明:碳化温度越高,得到的纱线表面越光洁,石墨化程度越高,电学性能也越好,1000℃碳化工艺得到的碳纳米纤维纱线电导率最高,为31.5 S/cm;与MnO 2复合后的碳纳米纤维纱线电导率大幅下降,当盐酸与高锰酸钾摩尔浓度比为4∶1时得到的复合纳米纤维纱线的电导率最高,为0.1200 S/cm。     

PAN基高性能碳纤维的制备及其性能的研究

碳纤维（简称ＣＦ）是一种新型高强度材料。本研究工作采取连续预氧化碳化方式，探索ＣＦ制备过程中工艺－结构－性能之间的关系。利用光学显微镜，密度，ｘ－射线衍射，元素分析等技术和测试手段重点研究工艺参数对ＣＦ结构性能的影响。实验结果表明，ＣＦ的结构性能与工艺条件有着密切关系，通过控制ＣＦ有关的制备工艺参数，可以制得高性能碳纤维。     

原子吸收分光光度法测定碳纤维中钾钠钙镁元素含量

碳纤维中的钾、钠、钙、镁元素的含量可用原子吸收分光光度法来测定。本文对酸性介质浓度以及干扰离子对测定结果的影响作了探讨,测定并比较了纯化处理前后的粘胶碳纤维以及几种不同纺丝法的聚丙烯腈原丝制成的碳纤维中钾、钠、钙、镁元素的含量。实验结果表明该法是一种快速、简便、准确、有效的方法。     

凝胶纺壳聚糖分散碳纳米管/聚丙烯腈纤维的研究

多壁碳纳米管(MWNTs)通过壳聚糖衍生物处理后与超高分子量聚丙烯腈进行复合,将得到的复合材料通过凝胶纺丝法制备出不同复合比例的MWNTs/聚丙烯腈纤维.将不同纺丝方法以及不同比例MWNTs对拉伸强度、模量、取向度、结晶结构的影响进行比较研究,同时通过电镜观察MWNTs的分散状况.结果表明:相比于湿法纺丝,通过凝胶纺丝法制备的复合纤维,MWNTs取向更好,分散更为均匀,纤维拉伸强度、模量都得到显著提高.对比未加MWNTs的对照样,在这个体系中加入质量分数为0.5%的MWNTs复合时,拉伸强度提高37%,弹性模量提高11.68%,并且声速取向度维持在相当高的水平(92.5%).     

Preparation of Si-doped and cross linked carbon nanofibers via electrospinning and their supercapacitive properties

In this work, Si-doped cross linked carbon nanofibers(Si/CNF) were prepared by electrospinning polyacrylonitrile(PAN) solutions containing polyhedral oligomeric silsesquioxane(POSS) as Si source, followed by thermal treatments. Scanning electron microscope(SEM) observations showed the smooth surfaces of pure PAN nanofibers, while PAN/POSS nanofibers with obviously rough or porous surfaces were obtained with relatively high POSS content. X-ray diffraction(XRD) identified the presence of POSS in the composite nanofibers. After thermal treatments, cross linked Si/CNFs with various morphologies were obtained. Energy-dispersive X-ray(EDX) and X-ray photoelectron spectroscopy(XPS) analyses confirmed the successful incorporation of Si into CNFs. Raman spectra suggested the degree of carbon ordering of Si/CNFs reduced slightly when compared with pure CNF. The obtained nanofibers exhibited typical performances of electric double-layer capacitors(EDLC).The specific capacitance of Si/CNF showed a moderate increase with POSS content and reached a maximum of175 F/g at 1 A/g with PAN:POSS equal to 100:5. Meanwhile Si/CNFs exhibited excellent cycling stability after1000 cycles. The influence of POSS on the capacitive performance might be attributed to the combined effects of evolution of morphology, conductivity and surface properties of Si/CNFs.     

A STUDY OF THE IMPOVEMENT OF TENACITY OF POLYACRYLONITRILE PREOXIDED FIBRE BY USING CUPROUS SALT

Polyacrylonitrile preoxided fibre PANOF is an intermediate in carbon fibre preparation. Thequality of PANOF is closely related to the property and structure of carbon fibre. In this paper, thermal mechanical analysis(TMA), thermogravimetric analysis(TGA), swell-ing differential scanning calorimetry(SDSC)and X-ray photoelectron spectroscopy(XPS)wereused to study the increase in tenacity of PANOF from the precursor treated with cuprous salt It has been discovered that the cuprous salt reacts strongly with the uncyclized CN of PANOF,resulting in an increase in the tenacity of PANOF by 30%. The results shwo that the cause of thistenacity improvement is the formation of coordinated complex. Cu~+is the central ion, and PANOFthe ligand. It is due to the coordinate bond that the network structure is formed from uncyclizedCN of PANOF. Therefore the tenacity of PANOF is remarkably increased.     

THE STRUCTURES OF SOME MESOPHASE PITCH-BASED CARBON FIBRES

The macro-and micro-structure of two groups(high modulus and high thermalconductivity)of MP-based carbon fibres were studied using X-ray diffraction,and both scanningand transmission electron microscopy.The dominant macrostructure in cross section is of foldedpseudo-radial layers which have a tendency to form a quasi-uniform domain as the fibre modulusincreases.It is found that high thermal conductivity fibres have both missimg sector and circularcross sections(possessed predominantly by the high modulus fibre group).The microstructuralstudy indicates that apart from the fibre C700,which has a three-dimensional graphite structure,these two groups of carbon fibres all exhibit a turbostratic stacking order.Furthermore it is foundthat the turbostratic stacking thickness as determined from dark-field measurement is much largerthan the classical crystallite thickness L_c as measured from X-ray diffraction.     

PAN大分子预氧化结构形成及演变机理

将聚丙烯腈（PAN）纤维在空气气氛中于130～190 ℃范围内进行热处理,通过傅里叶红外光谱（FT-IR）、凝胶渗透色谱（GPC）和元素分析（EA）等方法研究了PAN纤维预氧化初期的结构演变。结果表明：PAN大分子链中的羧酸共聚组分在130 ℃左右时引发分子内环化和分子间交联反应,生成酯羰基结构;随着热处理温度升高,PAN大分子进一步发生环化和脱氢反应,生成—C＝N—C＝N—共轭结构和—C＝C—C＝C—共轭结构;当温度高于190 ℃时,PAN大分子开始发生剧烈的环化脱氢反应,生成不饱和芳环结构。     

高锰酸钾改性活性炭的表征及其吸附Cu2+的性能

为提高活性炭对废水中Cu2+的去除效率,用不同浓度的KMnO4溶液,采用静置氧化/冷凝回流法对颗粒活性炭进行改性。采用BET,SEM,FT-IR和XRD等方法对改性活性炭的理化性质进行表征;探讨改性活性炭投加量、pH、吸附时间、温度对吸附Cu2+的影响。研究结果表明:当Cu2+质量浓度为20 mg/L,投加量为5 g/L时,0.01KMnO4-GAC和0.03KMnO4-GAC对Cu2+的吸附去除率分别达到84%和95%,分别是GAC的1.20和1.36倍;吸附剂在5 g/L投加量时,180 min基本达到吸附平衡;3种吸附剂对Cu2+的吸附,随着pH的降低而减少;温度对活性炭吸附Cu2+的影响相对较小。     

A12Of＋Cf／ZL109混杂复合材料的常温拉伸强度及预测模型

采用挤压铸造法制备了A12O3f， Cf／ZL109短纤维混杂金属基复合材料，并对该混杂复合材料的常温拉伸强度性能进行了实验及理论分析、在综合考虑纤维长度变化规律、两种纤维在拉伸过程中各自的行为和机理，以及热应力诱发位错强化和纤维弥散硬化等因素对复合材料强度影响的基础上。对复合材料强度预测的混合律模型加以发展和修正，建立了A12O3f， Cf／ZL109短纤维混杂复合材料的常温强度预测模型．利用该模型得到的理论预测值与实验值吻合较好．     

碳纤维表面处理及液相吸附性能

采用磷化物水蒸汽结合处理法，对低模量聚丙烯腈基碳纤维及粘胶基碳纤维进行了重量失损，液相吸附实验。对各种影响因素进行正交优化设计，平行实验和线性回归处理，以亚甲基半吸附量为指标，从而确定了最佳工艺参数，比表面、孔径公布和扫描电镜图片对活化前后的碳纤维结果地表征。     

共聚组分对聚丙烯腈(PAN)纤维预氧化程度的影响及其与碳纤维结构和性能的关联

利用自制碳纤维连续化试验线对两类聚丙烯腈（PAN）原丝进行了不同条件的梯度升温预氧化处理,并最终得到碳纤维。采用差示扫描量热分析（DSC）、红外光谱（FT-IR）、广角X射线衍射（WAXD）等表征手段分析了共聚组分对PAN分子链规整度的影响以及分子链规整度对预氧化、炭化过程中纤维结构转变的影响。结果表明,相对于三元共聚PAN纤维,二元共聚PAN纤维由于分子链规整度的提高,与环化反应有关的放热反应相对滞后发生;在相同的预氧化条件下,二元共聚PAN纤维能得到环化度较高的预氧化纤维,所得碳纤维的类石墨晶粒尺寸Lc也较大。结合碳纤维的拉伸强度和拉伸模量数据发现,二元共聚纤维适宜预氧化的温度要高于三元共聚纤维适宜预氧化的温度。     

金属离子对PAN基碳纤维结构和性能的影响

采用浸渍的方法,将钠、铁离子引入聚丙烯腈(PAN)纤维。经预氧化、低温碳化后,分别在1200、1300、1500℃温度下,对PAN纤维进行高温碳化处理。通过X射线衍射(XRD)、扫描电镜(SEM)、体密度、力学性能等测试手段研究了金属离子对PAN基碳纤维结构和性能的影响。结果表明,添加金属离子后,1500℃处理的碳纤维(002)面的层间距减小,碳纤维的抗拉强度降低,碳纤维的弹性模量增加;碳纤维横断面结构尺寸大小不一,结构疏松。金属离子的加入,一方面能促进碳纤维的乱层结构向石墨结构的转变,弹性模量增加;另一方面使碳纤维的缺陷增加,抗拉强度降低。     

基于多孔碳纳米微球的电化学传感器用于检测4-氨基苯酚

以多巴胺为前体,利用高温碳化的方法制备多孔碳纳米微球.多孔碳纳米微球通过透射电子显微镜和X射线粉末衍射图谱来进行表征.利用多孔碳纳米微球修饰玻碳电极,构建电化学传感器用于4-氨基苯酚的检测.结果表明,该传感器实现了对4-氨基苯酚的灵敏检测,线性检测范围为0.1~120μmol/L,检出限为20nmol/L.此外,该方法具有稳定性好、选择性高等优点.     

Preparation and thermal stability of zirconia-doped mullite fibers via sol-gel method

The zirconia-doped mullite fibers were prepared via a sol-gel method from aluminum isopropoxide-aluminum nitrate-tetraethyl orthosilicate system.The effects of zirconia doping on the sol spinnability,mullitization,structure and thermal stability of mullite fibers were investigated by means of Fourier transform infrared(FT-IR) spectroscopy,scanning electron microscopy(SEM) and X-ray diffraction(XRD).The results showed that Zr—O—C bond was presented with the involvement of zirconium acetate,which accelerat...