蜘蛛丝/聚-L-乳酸静电纺纤维束的形貌和力学性能

以1%(质量分数,下同)蜘蛛丝和9%聚-L-乳酸(PLLA)的混合液为纺丝溶液,采用静电纺丝方法制备了蜘蛛丝/PLLA复合纤维构成的连续纱线。探讨了纺丝温度、卷绕速度、后拉伸倍数等对纤维和纱线的形态结构及力学性能的影响。研究发现,加入蜘蛛丝蛋白后,PLLA复合纱线的强度提高了13%,纤维直径从1.1μm减小到了550nm;加热区温度为150℃时纱线强度最大;卷绕速度为(105±5)r/min时可以实现稳定纺丝;拉伸1.5倍时,纱线断裂强度和初始模量分别提高了66%和92%,断裂伸长率下降。     

Al-Ti合金钎焊SiC陶瓷接头界面微观结构与力学性能

SiC陶瓷具有优异的综合性能, 通过钎焊获得高强度接头是其获得广泛应用的重要前提。研究采用Al-(10, 20, 30, 40)Ti(Ti的名义原子含量10%、20%、30%、40%)系列合金, 在1550 ℃条件下, 对SiC陶瓷进行钎焊30 min。当中间层厚度为~50 μm时, SiC钎焊接头的平均剪切强度处于100~260 MPa范围内。当采用Al-20Ti合金作为钎料时, 随着中间层厚度从~100 μm减小至25 μm, 钎焊接头的平均强度逐渐提高, 且最大强度~315 MPa。同时, 钎焊中间层中(Al)相逐渐减少直至消失, 只留下Al₄C₃、TiC和(Al,Si)₃Ti相。SiC/Al-20Ti/SiC钎焊接头的断裂主要发生在靠近中间层/陶瓷界面位置的陶瓷基体内。     

纤维厚度和体积分数对压电纤维复合物应变性能的影响

实验制备了不同纤维厚度和体积分数的压电纤维复合物, 并在0.1 Hz的激励电压下测试了压电纤维复合物的自由应变性能和驱动性能, 研究复合物典型结构参数对其性能的影响。实验发现, 随着压电纤维厚度增加, 复合物自由应变和顶端位移下降, 1000 V激励电压下, 纤维厚度为200 μm样品纵向自由应变为665 με, 驱动Mylar膜产生的顶端位移为1.9 mm, 而纤维厚度为300 μm和400 μm样品的纵向自由应变仅为纤维厚度为200 μm样品的23.2%和11.7%, 顶端位移为纤维厚度为200 μm样品的45.8%和19.0%。压电纤维复合物具有驱动正交异性, 横向自由应变、纵向自由应变以及横向效应系数随着纤维体积分数的降低而减小, 纤维体积分数为74%的复合物其横向自由应变和纵向自由应变分别为体积分数为59%样品的2.04倍和1.72倍, 横向效应系数也从0.519减小到0.451。     

连续三叶形碳化硅纤维的性能研究

利用先驱体转化法制备三叶形 SiC纤维,并对纤维性能、电磁参数及其环氧基复合材料的力学性能等进行研究。结果表明三叶形 SiC纤维的异形度、当量直径有一定的分布;三叶形 SiC纤维增强复合材料的弯曲强度为 400MPa,弯曲模量为 30GPa,拉伸强度为425MPa,拉伸模量为 66GPa;电磁参数研究表明在x波段具有较好的频响特性;反射率测试表明,厚度为1.55mm时,在Ku 波段具有较好的吸波效果,反射衰减最大达-26dB。     

BN/SiC复合涂层改性炭纤维的吸波性能研究

以尿素、硼酸为原料, 采用浸涂工艺先在炭纤维表面制备BN涂层, 再以三氯甲基硅烷为前驱体, 采用化学气相沉积工艺在纤维表面沉积SiC涂层, 制得了BN/SiC复合涂层改性炭纤维。对BN/SiC复合涂层改性炭纤维的微观结构、抗氧化性能、介电性能及吸波性能进行了研究。结果表明: 炭纤维表面BN涂层的厚度约为0.1 μm, SiC涂层的厚度约为0.7 μm。炭纤维经表面BN/SiC复合涂层改性后, 抗氧化性能明显提高, 开始明显氧化失重温度从560℃提高到790℃, 最终氧化温度从780℃提高到1200℃以上; 且介电性能得到有效改善, 吸波性能显著提高。相比于未改性炭纤维, 厚度为2 mm的BN/SiC复合涂层改性炭纤维的最小反射率减小到-13.3 dB, 小于-10 dB的带宽增加至2.5 GHz。     

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。     

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

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。     

聚碳硅烷纤维的不熔化与SiC纤维制备研究

以聚二甲基硅烷(PDMS)为原料,在高压釜内高温高压反应制备了聚碳硅烷(PCS)先驱体,经熔融纺丝制备了PCS纤维,研究了在190 C下不同不熔化时间对PCS纤维氧化增重、Si-H键反应程度、凝胶含量、氧含量及最终SiC纤维氧含量与性能的影响.研究表明,在不熔化过程中,PCS结构中的Si-H键与氧反应,在PCS分子间形成Si-O-Si交联结构.随着不熔化时间的延长,PCS纤维发生氧化增重、Si-H键反应程度提高、凝胶含量增加,SiC纤维中氧含量也逐渐增加.在不熔化保温3h,制备的SiC纤维强度可达2.52GPa.随着不熔化时间的进一步延长,SiC纤维氧含量增加,其强度逐渐降低.     

含镁铝尖晶石的铝酸钙水泥的合成与流变特性

在1400℃和1500℃温度下合成了不同配比的铝酸钙水泥(CMA)。检测结果显示, 当温度升高时镁铝尖晶石的粒径由5 μm生长到15 μm。合成温度达到1400℃时, 镁铝尖晶石晶粒呈团簇状并分布在铝酸钙晶粒周围; 当合成温度升高至1500℃时, 镁铝尖晶石晶粒穿插在铝酸钙晶粒中。另外, 随着水泥中镁铝尖晶石含量的增加, 水泥的凝结时间延长, 同时粘度下降。相应的, 水泥储能模量和流动点的大小分别为0.15 MPa和4.44%。提高镁铝尖晶石相的含量或增大铝酸钙晶粒尺寸会减弱水泥水化时絮凝结构的强度。     

CVD-SiC界面改性涂层对气相渗硅制备C_f/SiC复合材料力学性能的影响

在气相渗硅制备C_f/SiC复合材料时,界面改性涂层非常重要。良好的界面改性涂层一方面起到保护碳纤维不受Si反应侵蚀的作用,另一方面起到调节纤维和基体界面结合状况。通过在C纤维表面制备CVD-SiC涂层来进行界面改性,研究CVD-SiC界面改性涂层对GSI C_f/SiC复合材料力学性能和断裂特征的影响,并分析其影响机制。结果表明:无CVD-SiC涂层改性的C_f/SiC复合材料力学性能较差,呈现脆性断裂特征,其强度、模量和断裂韧度分别为87.6MPa,56.9GPa,2.1MPa·m1/2。随着CVD-SiC涂层厚度的增加,C_f/SiC复合材料的弯曲强度、模量和断裂韧度呈现先升高后降低的趋势,CVD-SiC涂层厚度为1.1μm的C_f/SiC复合材料的力学性能最好,其弯曲强度、模量和断裂韧度分别为231.7MPa,87.3GPa,7.3MPa·m1/2。厚度适中的CVD-SiC界面改性涂层的作用机理主要体现在载荷传递、"阻挡"Si的侵蚀、"调节"界面结合状态3个方面。     

First principles calculations of thermal equations of state and thermodynamical properties of MgH2 at finite temperatures

We present the first principles calculations of the thermodynamical properties of magnesium hydride (MgH₂) over a temperature range of 0–1000 K. The phonon dispersions are determined within the density functional framework and are used to calculate the free energy of MgH₂ within the quasiharmonic approximation (QHA) at each cell volume and temperature T. Using the free energies the thermal equation of state (EOS) is derived at several temperatures. From the thermal EOS structural parameters such as the equilibrium cell volume (V₀) and elastic properties, namely, bulk modulus (K₀) and its pressure derivative are computed. The free energies are also used to calculate various thermodynamical properties within QHA. These include internal energy E, entropy S, specific heat capacity at constant pressure C_P, thermal pressure P_thermal(V, T) and volume thermal expansion ΔV/V (%). The good agreement of calculated values of S and C_P with experimental data exhibits that QHA can be used as a tool for calculating the thermodynamical properties of MgH₂ over a wide temperature range. P_thermal(V,T) increases strongly with T at all the volumes but it is a slowly varying function of volume for T = 298–500 K. According to Karki [B.B. Karki, Am. Miner. 85 (2000) 1447] such volume based variations can be neglected and so it is possible to estimate the thermal EOS only with the knowledge of the measured P_thermal(V, T) versus temperature at ambient pressure and isothermal compression data at ambient temperature. Temperature dependence of ΔV/V(%) shows that V₀ increased with increase in temperature. However, the percentage decrease in K₀ superseded this percentage increase in V₀ even at temperatures moderately higher than 298 K. Therefore, we suggest application of temperature (T > 298 K) as an approach to enhance the hydrogen storage capacity of MgH₂ because of its better compressibility at these temperatures.     

单模硫系玻璃光纤的制备及其超连续谱的产生特性

硫系玻璃具有独特的红外光学性能和极高的光学非线性等特点, 使得硫系光纤成为中红外超连续谱产生的优选材料。基于二次挤压法制备了单模As-S光纤, 并利用飞秒脉冲和光参量放大器作为泵浦源研究了该光纤的中红外超连续谱的产生特性, 包括光纤长度、泵浦波长、泵浦功率对超连续谱产生的影响。结果表明该单模光纤具有较低的传输损耗和较小的材料色散分布; 相比于传统零色散点波长附近泵浦, 在正常色散区且杂质吸收峰附近泵浦也可获得脉冲的极大展宽(泵浦参数: 4.5 μm, 1 kHz, 150 fs, 光纤长度23 cm, 输出谱宽为1.5~8.7 μm@60 dB带宽); 较短长度的硫系光纤便可产生超宽频谱输出, 相反, 光纤长度越长输出频谱越窄且平坦性变差。     

干法纺丝法制备低氧含量SiC纤维

通过粘度、凝胶含量和XRD等手段研究了聚碳硅烷(PCS)纺丝原液的干法纺丝性能和干纺PCS纤维的自交联过程, 并对所制得的低氧含量SiC纤维的组成、结构和性能进行了表征. 结果表明, PCS/二甲苯纺丝原液的最佳纺丝粘度范围在18.0～22.0Pa·s; 干纺PCS纤维在烧成温度超过250℃后开始发生自交联反应, 在烧成温度超过550℃后, 干纺PCS纤维完全交联形成了“不熔不溶”的网状结构; 干法纺丝法制备得到的SiC纤维与空气不熔化法制得的SiC纤维相比, 氧含量大幅降低, 仅在3.6wt%左右, 结晶度较高, 其耐高温抗氧化性也有明显的改善.     

Manufacture of High Performance Carbon Fibers from Precursors of Various Diameters

The effects of fiber diameter on the mechanical properties of PAN-based carbon fibers have been investigated in a series of processing experiments on fibers with different starting filament diameters. The fiber tows, with similar initial mechanical performance, were stretched at high temperatures to produce a large number of fiber types with a wide range of filament diameters. The three starting carbon fibers tows had nominal filament diameters of 5 μm, 6·5 μm, and 10 μm and contained 12000, 6000, and 3000 filaments respectively. These tows were stretched for 5 minutes at 2600^°C with a series of loads of up to 6 kg. For all fiber types and all stretching conditions, substantial increases in Young's moduli were induced, the increases being closely related to the induced extensions. However, it was found that tensile strengths generally decreased if fibers were subjected to high temperatures without significant stretching. On the other hand, the tensile strengths were restored to their original values when greater strains were induced by using higher stresses. Although fibers with a relatively large diameter of 8·3 μm were produced with a modulus of -470GPa and strength of -3·7 GPa, greater improvements in mechanical properties were achieved with smaller diameter fibers. The loads and temperatures involved in these hot stretching experiments were not excessive, and the investigations showed that serious consideration should be given to the feasibility of commercial production of high performance PAN-based carbon fibers by this processing route.     

(1-x)K0.48Na0.52NbO3-xBi0.45Nd0.05(Na0.92Li0.08)0.5ZrO3无铅压电陶瓷相结构及压电性能

为了在获得较高压电性能的同时又不大大降低陶瓷的居里温度(T_C), 设计和制备了Bi_0.45Nd_0.05(Na_0.92Li_0.08)_0.5ZrO₃改性的K_0.48Na_0.52NbO₃系无铅压电陶瓷((1-x)KNN-xBNNLZ), 研究了BNNLZ含量对KNN基无铅压电陶瓷相结构和电学性能的影响。研究结果表明, 所有陶瓷样品均具有较高的居里温度T_C(>300℃)。随着BNNLZ含量的增加, 陶瓷的正交-四方相变温度(T_O-T)不断向低温方向移动, 而三方-正交相变温度(T_R-O)不断向高温方向移动, 最终在陶瓷中形成了三方-四方(R-T)共存相, R-T共存相处于0.05<x<0.07范围。BNNLZ的加入引起陶瓷相结构的演化改变导致压电常数(d₃₃ )、介电常数(ε_r )、剩余极化强度 (P_r )和机电耦合系数(k_p )都先增大后减小, 当x=0.06时陶瓷具有最佳压电性能: d₃₃=313 pC/N, k_p=42%, P_r=25.48 μC/cm², ε_r=1353, tanδ=2.5%, T_C=327℃。     

低损耗As-S玻璃光纤的制备与应用研究

采用反复蒸馏提纯技术和开放式动态蒸馏相结合的工艺, 制备了高纯As-S玻璃, 基本消除了玻璃在2.9、4和6.3 μm处的杂质吸收。利用旋转法制备出壁厚均匀、表面质量优异的硫系玻璃套管。采用棒管法拉制出丝径50 μm, 芯径40 μm具有芯包结构的硫系玻璃光纤。拉制的As-S光纤机械性能和光学性能优异, 光纤丝径波动小于1%, 弯曲半径优于4 mm, 中红外波段损耗基线小于0.5 dB/m。制备出像元呈正方形排列, 出端规格64×9, 入端规格192×3, 用于线-面转换的红外传像束, 像束断丝率为2.7%。利用该异型传像束成功实现了长线阵的红外推扫成像。     

Processing and Characterization of Fiber Reinforced Intermetallic Matrix Composites

A series of intermetallic matrix composites reinforced with Al₂O₃ based fibers were fabricated by pressure casting. The Al₂O₃ based fibers used were DuPont's 20 μm diameter Fiber FP and PRD-166 fiber, Mitsui's 10 μm diameter Almax fiber, and Saphikon's 125 μm diameter single crystal Al₂O₃ fiber. The intermetallic matrices employed were alloys based on Ni₃Al, NiAl, Fe₃Al, Ti₃Al+TiAl, and Nb₂Al+NbAl₃. Optical, scanning and transmission electron microscopy were used to investigate the microstructure of the composites and the fibers. Tensile testing was conducted to determine the Weibull mean strength of the fibers in the as-received and heat treated conditions. The effect of fiber gage length on the Weibull mean strength of the PRD-166 and Fiber FP was evaluated. Indentation tests were performed to determine the effect of alloying additions on the fiber/matrix bond strength in shear in Saphikon fiber reinforced Ni₃Al composites.     

异型(三叶型)截面碳化硅纤维制备工艺研究

以聚碳硅烷（PCS）为原料,经不熔化和烧成制得三叶型碳化硅纤维,研究了纺丝温度,压力,收丝速度对纤维异形度和当量直径的影响,研究表明,较低的纺丝温度,适当高的纺丝压力和较低的转速有利于提高纤维的异形度,抗拉强度平均提高约30％。     

残余相和烧结温度对碳化硅陶瓷抗混酸腐蚀特性的影响

本工作主要研究了残余相和晶粒尺寸对碳化硅的抗混酸(HF-HNO₃)腐蚀特性。通过不同的烧结方法(固相烧结、液相烧结、反应烧结)制备出残余相不同的碳化硅材料。结果表明: 与液相烧结碳化硅(LPS SiC)和反应烧结碳化硅(RB SiC)相比, 固相烧结碳化硅(SSiC)具有更好的腐蚀抗性, 这是由于残余相石墨的抗腐蚀性强, 以及残余相在材料中形成不能相互联通的岛状结构。通过调节碳化硅的烧结温度, 可以影响材料中的晶粒尺寸, 研究结果发现相同烧结温度下随着残余相含量的增加, 材料腐蚀失重线性增加, 对曲线进行线性拟合, 其Y轴截距的绝对值代表不含碳的试样在该烧结温度下的腐蚀失重。研究表明随着烧结温度由2100℃升高到2160℃, 晶粒尺寸由2 μm增加到6 μm。此时其Y轴截距的绝对值分别为9.22(2100℃), 5.81(2130℃), 0.29(2160℃), 表明晶粒尺寸的增加有利于提高材料的抗腐蚀能力。     

Fine SiC fiber synthesized from organosilicon polymers: relationship between spinning temperature and melt viscosity of precursor polymers

A very fine silicon carbide (SiC) fiber with diameter of 6 m, about a half of that of a commercially available SiC fiber, was synthesized from a polymer blend of polycarbosilane (PCS) and polyvinylsilane (PVS). The fine SiC fiber was obtained by optimizing the composition and the spinning temperature of PCS-PVS polymer blends. In order to determine these optimum conditions, the relationship between temperature and melt viscosities of the polymer blends was investigated. As a result, it was found that the optimum spinning temperature range was within a temperature range where the melt viscosity is 5–10 Pa · s. Moreover, by blending PVS with PCS, the spinning temperature of the polymer blends was lowered, the spinnability of polymer system was improved, and finer polymer fiber was obtained compared with PCS. The optimum content of PVS in the polymer blend was 15–20 wt%.