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.     

含硼聚碳硅烷的制备及热解行为EI北大核心CSCD

为制备陶瓷产率高、高温性能优良的碳化硅(SiC)陶瓷先驱体,利用频那醇硼烷(PINB)与聚碳硅烷(PCS)的脱氢偶合反应,对聚碳硅烷进行化学改性。改变PINB与PCS的质量比(1∶20、1∶10、1∶5),制备了一系列不同硼(B)含量的含硼聚碳硅烷(PBCS)。通过傅里叶变换红外光谱分析、核磁共振氢谱分析、热重分析以及X射线衍射分析等手段研究了PBCS的组成、结构及热解行为。结果表明,通过B-H键的反应将B元素以PINB骨架形式引入PCS结构;引入B元素可以将PCS的陶瓷产率从78%提高至92%;另外,B元素的引入引起PCS的交联,PBCS的热解过程分3个阶段。同时B元素的引入抑制了SiC晶体的生长,将材料的耐温性能提高至1400℃。     

Mark Ⅲ型碳化硅纤维的研制

碳化硅(SiC)纤维是具有比强度高、比模最高、耐高温、抗氧化的新型增强材料。本文对 Mark Ⅲ型 SiC 纤维制备过程中聚二甲基硅烷、派松、聚碳硅烷的合成,聚碳硅烷纺丝、予氧化、高温烧成等工艺的原理、工艺参数和产物结构分析进行了讨论。     

低剂量γ射线辐射氧化法制备SiC纤维研究

空气气氛下采用γ射线辐射氧化联合热交联对聚碳硅烷(PCS)纤维进行了不熔化处理,并热解制备出SiC纤维。研究了辐射氧化、热交联及热解过程中PCS纤维的质量及形貌变化,对SiC纤维进行了分析测试。结果表明,吸收剂量为0.3MGy时可以制备出SiC纤维,吸收剂量为0.5MGy时获得的SiC纤维断裂强度达2.0GPa。利用该法制备的SiC纤维表面光滑,缺陷较少,结晶度较低,电阻率在103Ω·cm级。研究中PCS纤维的吸收剂量范围接近常规辐射加工剂量,具有实际应用价值。     

含乙烯基的聚碳硅烷的合成

利用聚碳硅烷与甲基乙烯基硅氮烷共混热聚反应 ,制得了含乙烯基的聚碳硅烷。分析了甲基乙烯基硅氮烷的结构 ,讨论了两者共热聚的反应过程 ,研究了制备条件对产物性能的影响。通过熔融纺丝制得了含不同乙烯基的适于电子束辐照的聚碳硅烷纤维。     

静电纺丝法制备SiC纤维

以聚碳硅烷(PCS)和聚乙烯吡咯烷酮(PVP)为原料制得前躯体溶液,采用静电纺丝法制备出PCS/PVP前驱体纤维,经高温分解得到SiC纤维.X射线衍射证实纤维中生成了立方结构β-SiC相.采用扫描电子显微镜(SEM)对前驱体纤维及煅烧后SiC纤维的形貌进行了观察,所制备的SiC纤维直径很小,但均匀性不是很高,且表面依附一层非晶形SiO2薄膜层.     

聚碳硅烷树脂性能及应用研究

合成了聚碳硅烷树脂,以该树脂为原料制备了SiC纤维。用电镜、红外光谱、X射线衍射、差热分析、热失重等方法对SiC纤维进行了研究,并对以聚碳硅烷树脂作为浸渍物质涂覆石墨进行了初步研究。     

固/液态聚碳硅烷共混制备碳化硅纤维的研究

以超支化液态聚碳硅烷(LPCS)与固态聚碳硅烷(纯PCS)的共混物作先驱体,熔融纺丝;所得原丝再在热空气气氛中氧化交联,在高温氮气气氛中热裂解,得到碳化硅纤维。研究表明,15%(质量分数)LPCS的加入,可使纯PCS先驱体的纺丝温度,从285℃降低到225℃;纺丝性能和纤维表面质量明显提高;还可以提高氧化交联的效率,降低交联温度,从而减少纤维部分融并、粘结的弊端;虽然纤维的室温力学强度有所降低,但抗氧化性能提高,1400℃氧化交联后,力学性能几乎不变;而纯PCS的力学性能却降为原来的50%。     

聚碳硅烷制备连续SiC纤维的不熔化处理工艺研究进展

综述了先驱体转化法制备SiC纤维过程中聚碳硅烷(PCS)的各种不熔化处理方式及其发展状况.通过不熔化方式对终烧产物SiC纤维性能的比较,讨论了各种不熔化方式的优缺点及其对SiC纤维中氧含量的影响,并指出了制备高性能SiC纤维不熔化技术研究的国内外差距及发展趋势.     

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.     

低能离子注入对聚吡咯甲烯的改性

利用低能氮离子对聚[(3乙酰基吡咯-2,5-二)对二甲氨基苯甲烯](Papdmabeq)薄膜进行了离子注入改性(注入能量为10～35 keV、剂量为1.2×1016～2.2×1017ions/cm2),研究了与材料三阶非线性极化率相关的物理量的变化规律.结果表明,氮离子注入使Papdmabeq薄膜的光电特性都发生了显著变化.适当能量和剂量的氮离子注入Papdmabeq薄膜后,薄膜中导电岛的数量增加,在聚合物分子链间形成了大的导电区域,导致其电导率显著提高.当注入离子的能量为25 keV、剂量为2.2×1017ionS/cm2时,Papdmabeq薄膜的电导率为9.2×10-4S/cm,比本征态Papdmabeq的电导率提高了5个数量级,且离子注入后薄膜电导率的环境稳定性优于经碘掺杂的Papdmabeq.氮离子注入可以使这种聚合物薄膜在可见光范围内的光吸收大幅度提高,使共轭程度得到显著增强.当注入离子的能量为35 keV、剂量为2.2×1017ions/cm2时,Papdmabeq的光学禁带宽度(Eg)由1.626 eV降低到1.340 eV.     

真空热循环对M40J/环氧复合材料力学性能的影响

分别测量了经不同次数单向真空热循环试验(93～413 K,10-5Pa)后M40J/5228A复合材料的拉伸强度、弯曲强度和层剪强度,研究了真空热循环对M40J/环氧复合材料力学性能的影响.结果表明,随着真空热循环次数的增加,90°和0°拉伸强度下降,并分别于48次和40次真空热循环后趋于平缓.弯曲强度随着真空热循环次数的增加表现出先上升后下降再趋于平缓的特征,而层剪强度变化不大.90°和0°拉伸强度的变化与界面脱粘程度密切相关.弯曲强度变化主要反映真空热循环时树脂基体后续固化效应的影响.层剪强度变化是界面脱粘与树脂基体后续固化两种因素综合作用的结果.     

Synthesis and up-conversion luminescence of Yb3 + –Ho3 + co-doped Na(Y1·5Na0·5)F6 nanorods

We present the optical up-conversion (UC) study for Yb^3?+?–Ho^3?+? co-doped Na(Y_1·5Na_0·5)F₆ nanorods synthesized by employing a facile hydrothermal method. Numbers of Ho^3?+? ion up-conversion emissions have been observed under 980 nm infrared diode laser excitation. Three UC emissions of interest, ultraviolet, violet and blue, are specially identified at 359, 387, 418 and 483 nm, corresponding to $^{5}{{G}}^{\prime}_{5}{/}^{3}\!{{H}}_{ 6}\to\ ^{ 5}\!{ {I}}_{ 8}$ , $^{ 5}\!{ {G}}_{ 4}{/}^{ 3}\!{ {K}}_{ 7}\to\ ^{ 5}\!{ {I}}_{ 8}$ , $^{ 5}{ {G}}_{ 5}\to$ $^{ 5}\!{ {I}}_{ 8}$ and $^{ 5}\!{ {F}}_{ 3}{/}^{ 5}\!{ {F}}_{ 2}{/}^{ 3}\!{ {K}}_{ 8}\to {}^{ 5}\!{ {I}}_{ 8}$ transitions, respectively. It is also found that the centre wavelength of blue UC emission shifts to 475 nm gradually as Ho^3?+? concentration decreases. Lastly, a brief analysis about UC mechanism is demonstrated according to the experimental results.     

The Influence of Oxygen/Argon Ratio on the Structure and Surface Morphology of GaBa2Cu3O7?δ Films Deposited by RF Magnetic Sputtering

$\mathrm{GaBa}_{2}\mathrm{Cu}_{3}\mathrm{O}_{7\mbox{-}\delta}$ thin films have been grown on CeO₂ cap layer by RF magnetic sputtering with different oxygen/argon partial pressure ratio from 2:1 to 1:5. The CeO₂ cap layers were fabricated by pulse laser deposition (PLD) on YSZ/CeO₂/Ni-5%W alloy substrate and had good properties in structure and surface morphology. We study the relationship between oxygen/argon ratio and the performance of the $\mathrm{GaBa}_{2}\mathrm{Cu}_{3}\mathrm{O}_{7\mbox{-}\delta}$ film in order to find out the optimized deposition condition. The structure and surface morphology of the $\mathrm{GaBa}_{2}\mathrm{Cu}_{3}\mathrm{O}_{7\mbox{-}\delta}$ thin films were measured by X-ray diffraction (XRD), Field emission scanning electron microscope (FE-SEM), Atomic force microscopy (AFM). It was found that the texture and surface performance of $\mathrm{GaBa}_{2}\mathrm{Cu}_{3}\mathrm{O}_{7\mbox{-}\delta}$ film, such as growth orientation, grain roughness, grain size and surface morphology, are deeply affected by the oxygen/argon ratio. And the film??s performance was the best when the oxygen/argon partial pressure ratio is 1:1.     

Photopyroelectric Calorimetry of \hbox {Fe}_{3}\hbox {O}_{4} Magnetic Nanofluids: Effect of Type of Surfactant and Magnetic Field

Five types of magnetic nanofluids, based on \(\hbox {Fe}_{3}\hbox {O}_{4}\) nanoparticles with water as the carrier liquid, were investigated by using the two photopyroelectric (PPE) detection configurations (back (BPPE) and front (FPPE)), together with the thermal-wave resonator cavity (TWRC) technique as the scanning procedure. The difference between the nanofluids was the type of surfactant: double layers of lauric (LA–LA), oleic (OA–OA), and miristic (MA–MA) acids and also double layers of lauric–miristic (LA–MA) and palmitic-oleic (PA–OA) fatty acids were used. In both detection configurations, the information was contained in the phase of the PPE signal. The thermal diffusivity of nanofluids was obtained in the BPPE configuration, from the scan of the phase of the signal as a function of the liquid’s thickness. Using the same scanning procedure in the FPPE configuration, the thermal effusivity was directly measured. The influence of a 0.12 kG magnetic field on the thermal effusivity and thermal diffusivity was also investigated. Because of different surfactants, the thermal effusivity of the investigated nanofluids ranges from \(1530\,\hbox {W}\cdot \hbox {s}^{1/2} \cdot \hbox { m}^{-2}\cdot \hbox { K}^{-1}\) to \(1790\,\hbox { W}\cdot \hbox {s}^{1/2}\cdot \hbox { m}^{-2}\cdot \hbox { K}^{-1}\) , and the thermal diffusivity, from \(14.54~\times ~10^{-8}\,\hbox { m}^{2}\cdot \hbox { s}^{-1}\) to \(14.79~\times ~10^{-8}\,\hbox { m}^{2}\cdot \hbox { s}^{-1}\) . The magnetic field has practically no influence on the thermal effusivity, and produces a maximum increase of the thermal diffusivity (LA–LA surfactant) of about 4 %.     

Thermal Conductivity and Raman Spectra of Carbon Fibers

Due to its unique physical properties, carbon fiber (CF) has been widely studied for extensive application in aerospace and machinery. In this study, the thermal diffusivity of three kinds of CF sample is characterized by the transient electrothermal technique at room temperature. By subtracting the effect of radiative losses, the effective thermal diffusivity of CFs can be calculated as \(6.46\times 10^{-6}\,\hbox {m}^{2}\cdot \hbox {s}^{-1}\), \(6.58\times 10^{-6}\,\hbox {m}^{2}\cdot \hbox {s}^{-1}\) and \(2.01\times 10^{-4}\,\hbox {m}^{2}\cdot \hbox {s}^{-1}\), respectively. For the first time, the emissivity coefficient of carbon fiber is calibrated as 0.78. Combined with Raman spectra and phonon scattering, we found that the better crystalline structure and low defect in CF have an obvious impact on its thermal diffusivity.     

Surface Recombination Velocity Dependence on Morphological Properties of CdTe Thin Films Prepared by Close-Spaced Sublimation

Cadmium telluride (CdTe) thin films were prepared on glass substrates by employing the close-spaced sublimation technique. Different source ( $T_\mathrm{sou}$ ) and substrate temperatures ( $T_\mathrm{sub}$ ) were used in order to change the structural properties of layers. The ranges chosen were: $550\,^{\circ }\hbox {C} \le T_\mathrm{sou} \le 650\,^{\circ }\hbox {C}$ and $400\,^{\circ }\hbox {C} \le T_\mathrm{sub} \le 600\,^{\circ }\hbox {C}$ . The environment in the growing chamber was also changed with the purpose to study its influence on the crystalline properties of the surface and volume of the material. Three different surroundings were used: vacuum, high-purity argon, and high-purity oxygen. The surface recombination velocity (SRV) was calculated from photoacoustic (PA) measurements by employing the open PA cell configuration. The behavior of the experimental results was analyzed as a function of the structural characteristics of the films: texture and grain size. Scanning electron microscopy, optical absorption, X-ray diffraction, and dark resistivity measurements were also employed to analyze the properties of the CdTe films. The minimum value for the SRV was found for $T_\mathrm{sou} = 650\,^{\circ }\hbox {C},\, T_\mathrm{sub} = 600\,^{\circ }\hbox {C}$ in an oxygen ambient.     

Magnetic Properties of Nanocrystalline Nickel–Cobalt Ferrites (\mathrm{Ni}_{1/2}{\mathrm{{Co}}}_{1/2}{\mathrm{{Fe}}}_{2}{\mathrm{O}}_{4})

In this study, the nanocrystalline nickel–cobalt ferrites $(\mathrm{Ni}_{1/2}\mathrm{Co}_{1/2}\mathrm{Fe}_{2}\mathrm{O}_{4})$ were prepared via the citrate route method at $27\,^{\circ }\mathrm{C}$ . The samples were calcined at $300\,^{\circ }\mathrm{C}$ for 3 h. The crystalline structure and the single-phase formations were confirmed by X-ray diffraction (XRD) measurements. Prepared materials showed the cubic spinel structure with m3m symmetry and Fd3m space group. The analyses of XRD patterns were carried out using POWD software. It gave an estimation of lattice constant “ $a$ ” of 8.3584 Å, which was in good agreement with the results reported in JCPDS file no. 742081. The crystal size of the prepared materials calculated by Scherer’s formula was 27.6 nm and the electrical conductivity was around $10^{-5}~\mathrm{S}\,\cdot \, \mathrm{m}^{-1}$ . The permeability component variations with frequency were realized. The magnetic properties of the prepared materials were analyzed by a vibrating sample magnetometer (VSM). It showed a saturation magnetization of $27.26\,\mathrm{emu} \cdot \mathrm{m}^{-1}$ and the behavior of a hard magnet.     

Effect of CTAB coating on structural,magnetic and peroxidase mimic activity of ferric oxide nanoparticles

In the present work, pristine and cetyl trimethyl ammonium bromide (CTAB)-coated ferric oxide nanoparticles \((\hbox {CTAB@Fe}_{2}\hbox {O}_{3} \hbox { NPs})\) were synthesized and studied as enzyme mimics. The w/w ratio of \(\hbox {Fe}_{2}\hbox {O}_{3}\) to CTAB was varied as 1:1 and 1:2. Transmission electron microscopic analysis revealed that pristine NPs had an average size of 50 nm, whereas the presence of CTAB resulted in the formation of nanorods with length of 130 nm. BET studies confirmed enhancement of surface area on CTAB coating, which was maximum for w/w ratio 1:1. The synthesized pristine NPs and CTAB-coated NPs were evaluated for their peroxidase mimic activity using o-dianisidine dihydrochloride as substrate. Optimum pH, temperature, substrate and NPs concentration for the reaction were 1, \(25^{\circ }{\mathrm{C}}\), \(0.16~\hbox {mg}~\hbox {ml}^{-1}\) and \(1~\hbox {mg}~\hbox {ml}^{-1}\), respectively. Peroxidase mimic activity of \(\hbox {CTAB@Fe}_{2}\hbox {O}_{3}\hbox { NPs}\) (w/w 1:1) was higher than that of pristine NPs. However, further increase in CTAB coating (w/w 1:2) resulted in lowering of peroxidase mimic activity. Kinetic analysis was carried out at optimized conditions; maximum velocity (\(V_{\mathrm{max}})\) and Michaelis constant (\(K_{\mathrm{m}})\) value of \(\hbox {CTAB@Fe}_{2}\hbox {O}_{3}\hbox { NPs}\) at 1:1 w/w ratio were 7.69 mM and \(1.12~\upmu \hbox {mol}~\hbox {s}^{-1}\), respectively.     

A Novel Vibrating Finger Viscometer for High-Temperature Measurements in Liquid Metals and Alloys

A novel vibrating finger viscometer for high-temperature measurement in liquid metals and alloys up to 1823 K was constructed. The dynamic viscosity (\(\eta \)) of the liquid fluid is measured as a product of \((\rho \cdot \eta )^{0.5}\) and the relative change of the field coil input for a constant amplitude recording at the resonant frequency of the oscillator. The viscometer was calibrated at 298 K using reference silicon oils with varying kinematic viscosities (\(\nu \)), \((0.79\hbox { to } 200)\times 10^{-6}\hbox { m}^{2}\cdot \hbox {s}^{-1}\). In the present study, the viscosity of liquid gold (\(99.99\,\%\) Au), silver (\(99.9\, \%\) Ag), and tin (\(99.9\,\%\) Sn) was measured. The viscosities expressed as an Arrhenius function of temperature are:

$$\begin{aligned} \hbox {for Au:}\quad \quad \hbox {ln }\eta= & {} -0.1990+\frac{2669}{T}\\ \hbox {for Ag:} \quad \quad \hbox {ln }\eta= & {} -0.4631+\frac{2089}{T}\\ \hbox {for Sn:} \quad \quad \hbox {ln }\eta= & {} -0.5472+\frac{671}{T} \end{aligned}$$

The viscosity values are consistent within the range of available literature data.