聚丙烯腈/石墨烯纳米复合物的制备、表征及其热性能

采用以水和N,N-二甲基甲酰胺的混合溶剂作反应介质的沉淀聚合法制备了聚丙烯腈/石墨烯纳米复合物。利用傅里叶红外光谱(FT-IR)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)和广角X射线衍射(XRD)研究了聚丙烯腈/石墨烯复合物的组成、结构、形貌及两组份的相互作用。利用差式扫描量热分析(DSC)研究了聚丙烯腈及纳米复合物的热性能。结果表明,强极性的聚丙烯腈与石墨烯之间存在较强的非共价相互作用;由于石墨烯的加入,聚丙烯腈的玻璃化转变温度提高了30℃;石墨烯添加量为3%(质量分数)时,聚丙烯腈在氮气和空气中的环化反应放热峰值分别提高了3和11℃;石墨烯使聚丙烯腈在热稳定化过程中的环化反应和氧化反应放热峰宽化、缓和。     

木质素-丙烯腈共聚物纤维热稳定化过程中的直径尺寸效应EI北大核心CSCD

通过酯化反应和自由基共聚反应制备了具有良好可纺性的木质素-丙烯腈(LS-AN)共聚物,采用湿法纺丝工艺制备了3种不同直径的LS-AN共聚物纤维,然后在梯度升温模式下对其进行热稳定化处理,采用差示扫描量热仪、红外光谱仪、密度梯度仪研究了LS-AN共聚物纤维热稳定化过程中的直径尺寸效应。结果表明:在空气气氛中,减小直径能够显著促进热稳定化反应的进行;减小纤维直径有利于氧向纤维内部扩散,促进氧化反应的进行,从而获得均质的径向稳定化结构;减小纤维直径可以显著提高碳纤维的力学性能,由直径最小的LS-AN共聚物纤维制得了拉伸强度和拉伸模量分别达到849 MPa和146GPa的碳纤维。     

热稳定化过程中PAN纤维热应力与热化学反应的关联性

借助DSC、FTIR、EA、WAXD和热应力变化等表征手段,系统研究了六种聚丙烯腈（PAN）纤维在热稳定化过程中应力变化特征与纤维热化学反应的内在关联.结果表明：在热稳化定化过程中PAN纤维化学应力峰的起始温度和峰顶温度很好地对应了纤维DSC起始与峰顶的温度,因而可采用化学热应力表征PAN纤维环化的反应速率和程度.由于化学应力峰的变化与PAN大分子的组成、有序度、芳构化指数以及密度等特征结构参数的变化具有较紧密对应关系,意味着热应力可用于连续热稳定化过程中在线控制纤维的结构.     

PAN纤维热稳定化过程中环化反应对氧化反应的影响

在惰性气氛中制备了不同环化程度的聚丙烯腈(PAN)热稳定化纤维,并将其在含氧气氛中进一步氧化处理,通过差示扫描量热仪(DSC)、傅立叶变换红外(FT-IR)和元素分析(EA)等方法研究了PAN纤维热稳定化过程中环化反应对氧化反应的影响。结果表明,与环化反应相比,氧化反应可在更低的温度下进行;对于环化程度越高的PAN热稳定化纤维,在含氧气氛中经相同条件热处理后氧含量越高,即氧化反应程度越高,故环化反应对氧化反应具有促进作用。     

热氧稳定化过程温度效应对PAN纤维径向氧元素扩散速率的作用

在梯度升温和恒温两种模式下,对聚丙烯腈（PAN）纤维进行了热氧稳定化处理,借助FTIR、核磁共振碳谱（13 C-NMR）、元素分析（EA）、DSC、X-射线能谱（EDS）、密度等多种表征手段系统研究了不同温度下热氧稳定化纤维皮-芯结构的形成机制和氧元素的扩散速率。研究结果表明：氧化反应速率小于氧的扩散速率时,PAN纤维...     

热氧稳定化过程中聚丙烯腈纤维序态结构的变化

研究了聚丙烯腈(PAN)共聚纤维在连续热氧稳定化过程中序态结构的变化,结果表明:X射线衍射极图所提供的0°-360°全角扫描信息,可表征纤维内部晶面法向分子链的分布密度,描述分子链取向结构的变化程度;可较全面.动态和直观地解析聚丙烯腈大分子链在热氧稳定化过程中经历的由初期取向结构改善到中、后期大分子链解取向的全过程.在较低的热氧稳定化温度下,PAN大分子链无序区先发生化学反应,有序度变化不大;当热处理提供的能量超过有序区环化和改变分子构象所需要的能量时,有序区发生剧烈的热化学反应,有序度急剧下降.     

250℃下时间效应对PAN纤维热氧稳定化反应的影响及关联

借用傅里叶变换红外光谱(FT-IR)、元素分析(EA)、X射线衍射(XRD)和示差扫描量热分析(DSC)等手段,对比研究了热氧稳定化过程中250℃下时间效应与两种聚丙烯腈(PAN)共聚纤维及其炭纤维结构和性能之间的关联。研究结果表明,PAN纤维在250℃温区内停留超过9min时,最终热氧稳定化纤维的环化度(RCI)、体密度和芳构化指数(AI)的增加速率开始变小;炭纤维的孔含量(Vp)值与内部微晶的d002值开始增大,微晶排列的规整程度变差,缺陷增多,拉伸强度开始降低。     

热双金属的稳定化热处理

文中阐述了稳定化热处理对热双金属元件应用的重要性。介绍了对 5J11、5J16、5J18和R25进行不同稳定化热处理的试验结果.     

高分子量聚丙烯腈纤维热稳定化过程中结构及性能演变

为了研究预氧化工艺对高分子量聚丙烯腈纤维结构和性能的影响,分别利用FTIR、广角X射线衍射仪、差式扫描量热仪及单丝强度细度仪等表征手段,通过对不同预氧化温度和时间下纤维的化学组成、晶体结构的演变、热稳定性、拉伸强度和模量的变化的研究,考察了预氧化工艺对纤维结构及性能演变的影响。研究发现,随着热稳定化温度的升高或稳定时间的延长,纤维原先线性分子链转变成环状结构部分增加,氰基组分残留率降低,纤维整体结晶度下降,结晶尺寸减小,热稳定性和碳化收率增加,纤维强度、模量逐渐降低。     

聚丙烯腈热稳定化纤维的裂解行为

在聚丙烯腈基碳纤维(PANCF)制备过程中会有40%~50%的质量损失,主要发生在300~800℃范围内。对PAN裂解失重行为的研究有利于理解PANCF类石墨结构的形成机理,为制备高性能碳纤维和提高碳化收率提供理论依据。通过热重分析法(TGA)模拟PAN纤维的裂解失重过程,结果表明:在空气中进行稳定化的纤维主要有两个阶段的裂解,分别受腈基的环化率和氧含量控制。环化率和氧含量通过影响裂解行为在碳纤维中形成的缺陷结构,最终影响碳纤维的致密性。环化率越高,形成的缺陷结构越少,碳纤维的致密性越好;相反氧含量越高,形成缺陷结构越多,碳纤维的致密性越差。     

低电阻率Si-C-O纤维制备——聚合物原丝的不熔化处理

采用聚二甲基硅烷 (PDMS)与不同比例的聚氯乙烯 (PVC)共裂解合成制备富碳Si C O纤维先驱体聚合物 .经熔融纺丝制成聚合物原丝。通过热分析、红外光谱研究了聚合物原丝的空气不熔化处理机理。结果表明 :聚合物原丝的不熔化机理与纤维的组成有关。考察了不熔化温度、时间及升温速率等因素对纤维不熔化处理的影响。     

直链脂肪酸镧对PVC的热稳定作用

制备了几种常见的直链脂肪酸镧,采用刚果红法对PVC进行了热稳定测试,并通过红外光谱分析对直链链脂肪酸镧的热稳定机理进行了探讨。结果表明,长链脂肪酸镧对PVC的热稳定作用顺序为月桂酸镧>肉豆蔻酸镧>硬脂酸镧>棕榈酸镧>癸酸镧。随分子链长度的减小,对PVC的热稳定作用下降,同时还受到镧元素含量的影响。通过红外光谱分析,推测直链脂肪酸镧对PVC的热稳定机理为:脂肪酸镧在和PVC共同受热的过程中,镧与PVC链段中不稳定的氯容易发生配位反应,减弱了C-Cl键的极性和β-H的酸性;同时会吸收PVC分解的HCl。     

Thermal stability of β-tricalcium phosphate doped with monovalent metal ions

The effect of doping β-tricalcium phosphate with monovalent metal ions (lithium, sodium, and potassium ions) on its thermal stability was evaluated using the formation ratio of α-tricalcium phosphate and the rate constant for β-α transformation. The thermal stability of β-tricalcium phosphate doped with monovalent metal ions was higher than that of pure β-tricalcium phosphate, and increased with the amount of metal ions. The increase in stability was attributed to the occupation of all calcium sites including vacancy in β-tricalcium phosphate structure by the calcium ions and monovalent metal ions and the resultant crystal stabilization. However, the thermal stability of β-tricalcium phosphate doped with monovalent metal ions was lower than that of β-tricalcium phosphate doped with magnesium ions. These results indicate that the thermal stability of β-tricalcium phosphate is influenced by the difference in the structural stabilization caused by doping metal ions into different calcium sites in the crystal structure.     

Ordering and stabilization in quenched CuAlNiMnB alloys

The ordering and stabilization behaviour of a set of CuAlNi alloys with manganese and boron additions have been studied. Specimens were subjected to different thermal treatments, mostly consisting of a direct quench into martensite from different temperatures. The transformation was studied by differential scanning calorimetry, and X-ray diffraction was also used to check the martensite and parent phase structures. According to the results, the first reverse transformation after quenching into martensite stems from two competitive processes, namely the stabilization of the martensite and a decrease of the transformation temperatures due to quenched disorder. The temperature from which the quench is performed is the critical parameter determining whether stabilization or disorder suppression predominates. The degree of stabilization increases with the manganese content.     

丙烯酸酯类抗氧剂对聚酰胺的热氧稳定作用

采用丙烯酸酯类抗氧剂AL与主、辅抗氧剂复合构成三元复合稳定体系,利用其双官能团稳定机理,捕获聚合物降解产生的碳自由基,以进一步提高尼龙6热氧稳定性能。研究了抗氧剂AL对尼龙6的热氧稳定作用,结果表明,在130℃长期热氧老化过程中,抗氧剂AL的加入能有效抑制尼龙6黏度和分子量的降低,抑制其端羧基形成和含量的增加,提高尼龙6的热分解温度,并能有效延缓尼龙6冲击韧性的下降,获得较高的保留率。     

Application of a Heat Hydraulic Accumulator to Thermal Stabilization of the Evaporation Zone of a Heat Pipe

The use of a heat hydraulic accumulator (HHA) for thermal stabilization of the evaporation zone of a heat pipe (HP) has been proposed. The experimental setup for investigation of the heat pipe with a heat hydraulic accumulator has been described. Results of the experiments on this assembly have been presented. It has been shown that the installed heat hydraulic accumulator allows thermal stabilization of the evaporation zone of the heat pipe to a precision of 1°C.     

铜基形状记忆合金耐热稳定性的研究

综述了铜基形状记忆合金耐热稳定性(热弹性马氏体的稳定化、母相时效效应、热循环效应)，以及提高铜基形状记忆合金耐热稳定性的途径。     

A strategy for designing stable nanocrystalline alloys by thermo-kinetic synergy

Aiming to design stable nanocrystalline(NC) materials, so far, it has been proposed to construct nanostructure stability maps in terms of thermodynamic parameters, while kinetic stabilization has seldom been considered, despite the synergy of thermodynamics and kinetics. Consequently, the thermodynamically stabilized NC materials may be easily subjected to grain growth at high temperatures due to the weakly kinetic stabilization. Starting from the thermo-kinetic synergy, a stabilization criterion is proposed as a function of intrinsic solute parameters(e.g. the activation energy for bulk diffusion and the segregation enthalpy), intrinsic solvent parameters(e.g. the intrinsic activation energy for GB migration and the GB energy) and processing parameters(e.g. the grain size, the temperature and the solute concentration). Using first-principles calculations for a series of combinations between fifty-one substitutional alloying atoms as solute atoms and Fe atom as fixed solvent atom, it is shown that the thermal stability neither simply increases with increasing the segregation enthalpy as expected by thermodynamic stabilization, nor monotonically increases with increasing the activation energy for bulk diffusion as described by kinetic stabilization. By combination of thermodynamic and kinetic contributions, the current stabilization criterion evaluates quantitatively the thermal stability, thus permitting convenient comparisons among NC materials involved by various combinations of the solute atoms, the solvent atoms, or the processing conditions. Validity of this thermo-kinetic stabilization criterion has been tested by current experiment results of Fe-Y alloy and previously published data of Fe-Ni, Fe-Cr, Fe-Zr and Fe-Ag alloys,etc., which opens a new window for designing NC materials with sufficiently high thermal stability and sufficiently small grain size.     

Subnanometric stabilization of plasmon-enhanced optical microscopy

We have demonstrated subnanometric stabilization of tip-enhanced optical microscopy under ambient condition. Time-dependent thermal drift of a plasmonic metallic tip was optically sensed at subnanometer scale, and was compensated in real-time. In addition, mechanically induced displacement of the tip, which usually occurs when the amount of tip-applied force varies, was also compensated in situ. The stabilization of tip-enhanced optical microscopy enables us to perform long-time and robust measurement without any degradation of optical signal, resulting in true nanometric optical imaging with high reproducibility and high precision. The technique presented is applicable for AFM-based nanoindentation with subnanometric precision.