多孔碳化硅及氧化铝/碳化硅复合膜的制备与性能

以碳化硅(SiC)为骨料,氧化铝(Al2O3)为烧结助剂,在空气气氛下反应烧结制备碳化硅多孔陶瓷支撑体,并配制Al2O3制膜液,采用浸浆法在支撑体表面进行涂膜.重点考察Al2O3添加量对支撑体的孔隙率、抗弯强度、微观形貌的影响与支撑体的抗热震性能;采用环境扫描电镜(SEM)观察膜层的微观形貌,并对膜层的气体渗透性能、抗热震性能等进行考察.结果表明,当烧结温度为1500℃、Al2O3添加质量数为10%时,支撑体的抗弯强度为31MPa、孔隙率为30%,气体渗透系数为4 000m3/(m2.h.0.1MPa),抗热震性能良好;制备的碳化硅陶瓷复合膜,其平均孔径为4.7μm,膜厚为110μm,气体渗透系数为1 917m3/(m2.h.0.1MPa),具有良好的抗热震性能.     

碳掺杂对碳化硅膜支撑体结构与性能的影响

以200μm碳化硅为骨料,氧化锆为烧助剂,莫来石纤维为增强剂,碳粉为造孔剂,经过混合造粒后干压成型制得生坯,然后通过高温原位反应烧结获得大孔径、高孔隙率的SiC膜支撑体.本文主要考察了造孔剂碳粉粒径和含量对SiC膜支撑体性能的影响,并测试膜支撑体的高温抗热震性能和高温热膨胀特性.研究结果显示,当碳粉粒径和质量分数分别为20μm和15%,烧结温度1 450℃,保温时间为4 h时,制备的碳化硅支撑体有较好的综合性能,支撑体抗折强度达24 MPa,开口孔隙率为42.5%,平均孔径50.5μm,1 kPa压力下气体流量达到1 400 m~3/(m~2·h).SiC膜支撑体热膨胀系数为5.0×10~(-6) K~(-1),并在30～800℃下连续冷热循环60次以上,仍然保持较高的抗折强度,是较好的高温气体过滤材料.     

亲水性高分子-陶瓷复合膜的制备与表征

采用均质的氧化铝支撑体和不同表面层孔径的非对称氧化铝支撑体直接接枝聚丙烯酸(PAA)制备亲水性PAA-Al2O3复合膜。对所制备出复合膜的红外光谱(IR)分析、光电子能谱(XPS)分析、扫描电子显微镜(SEM)分析和表面的水接触角分析表明,成功地制备出了PAA-Al2O3复合膜。在相同实验条件下对所制备的复合膜进行纯水和纯乙醇的通量实验以及质量分数95%乙醇的脱水分离试验表明,最适合用于制备PAA-Al2O3复合膜的陶瓷膜支撑体是孔径为2～3μm的均质氧化铝支撑体,用其制备的复合膜的分离因子为139.33,通量为0.61kg/(m2.h),可以达到分离效率高、通量较大的效果.     

改进浸浆法制备氧化钛/多孔钛复合微滤膜

金属陶瓷复合膜以多孔金属为载体、多孔陶瓷为活性分离层,结合了陶瓷膜和金属膜的优点,具有良好的工业应用前景。采用改进浸浆法制备氧化钛/多孔钛复合微滤膜。将氧化钛粉体分散到氧化钛溶胶中作为制膜液,以提高制膜液在多孔金属支撑体表面的润湿性.结果表明,相同温度下溶胶的表面张力远小于水的表面张力,溶胶分散制膜液的表面张力也远小于水分散制膜液的表面张力.由此明显地改变了制膜液和支撑体的润湿性能,从而可以制备得到连续完整的膜层.由于溶胶粒子对粒径较大的氧化钛颗粒的烧结促进作用,使得膜层可以在较低的温度下烧结.在850℃下烧结的膜层平均孔径为0.31μm,且分布较窄.膜层表面完整无缺陷,与支撑体结合情况良好,膜层厚度约为17μm.膜层N2渗透通量为6.6×105L/(m2.h)(0.1 MPa).     

粗细粉混用法制备堇青石膜支撑体

将粒径分别为1.5和25μm的堇青石粉体按一定比例球磨混匀,添加适当的粘结剂和造孔剂,经捏合、陈腐、挤出成型及烘坯处理后,程序升温至一定温度烧结2h制备膜支撑体.结果表明,细粉含量20%(质量分数)、1400℃烧结所得的支撑体综合性能较好:钝水通量为10.3m3/(m2·h);爆破压力为2.21MPa.其浸渍于5%(质...     

泥浆喷涂制备阳极支撑YSZ电解质薄膜工艺研究

采用泥浆喷涂工艺制备SOFC用阳极支撑YSZ电解质薄膜,首先采用模压成型工艺制窷iO-YSZ阳北极基底,通过优化泥浆制备工艺条件及喷涂条件,在NiO-YSZ阳极基底上喷涂均匀平整的YSZ电解质涂层,进一步采用共烧结工艺使YSZ电解质层致密.通过在基底中添加碳粉造孔剂,调节阳极基底的烧结收缩率与电解质层烧结收缩率一致,避免电解质涂层的开裂和变形.阳极基底中加入5wt%含量的碳粉,阳极与电解质层烧结收缩率一致.扫描电子显微镜观察电解质涂层表面形貌表明,球磨24h的泥浆喷涂的YSZ涂层较好,阳极基底与电解质膜在1400℃烧结2h,电解质膜层致密,表明通过泥浆喷涂工艺可以制备出致密电解质层.     

NaA分子筛合成残余物掺杂制备SiC膜支撑体

选用平均粒径100μm碳化硅为主要原料粉体,NaA分子筛合成废液中提取的粉体(主要成分为NaA分子筛和微量硅铝钠化合物)为烧结助剂,采用挤出法进行生坯成型,最后通过原位烧结技术制备高温气体净化用的管式碳化硅膜支撑体(外径60 mm,内径40 mm,长1 500 mm).研究结果表明,烧结助剂的最佳含量为质量分数3%,随着烧成温度的升高,碳化硅膜支撑体孔隙率逐渐减小,平均孔径也随之增加.当烧成温度达到1 150℃时,膜支撑体平均孔径为30.92μm,气体通量为99.32 m~3/(m~2·h·kPa),抗弯强度达到29.50 MPa,同时也表现出优异的抗热震性能和耐酸腐蚀性能,为高温气体净化碳化硅膜的低成本、绿色化制备以及应用研究提供了理论依据.     

钇稳定氧化锆纳米粉体烧结工艺的研究

实验研究了钇全稳定氧化锆(8YSZ)纳米粉体的烧结工艺,根据阿基米德原理测瓷体密度,通过测定烧结前后瓷片尺寸获得烧结线收缩率,使用扫描电子显微镜观测样品微观形貌,并探讨了纳米粉体烧结的致密化过程,分析了烧结工艺对致密度和晶粒大小的影响,得到了8YSZ纳米粉体合理的烧结工艺为:采用两步烧结,首先升温到1500℃,升温速率为3℃/min,然后降低温度到1450℃,烧结时间为4h.结果显示,采用该工艺,可以得到相对密度98%,晶粒尺寸小于3μm的性能优异的8YSZ瓷体.研究发现,粉体粒度对烧结性能影响较大,纳米粉体比普通粉体具有较低的开始烧结温度,双粒度混合粉体可以进一步提高其烧结性能.     

掺入Al_2O_3对固体氧化物电解质材料YSZ性能影响的研究

在立方相的钇稳定化氧化锆 [(ZrO2 ) 0 .92 (Y2 O3) 0 .0 8](YSZ)中 ,掺入少许不同量的Al2 O3,研究其对基体材料YSZ的烧结性能、机械强度和导电性能的影响 ,并对其机理进行了分析。实验结果表明 ,掺入Al2 O3能够明显降低电解质烧结温度 ,改善烧结性能。在 130 0℃烧结 1h后 ,少量掺杂Al2 O3的样品晶粒尺寸明显比纯YSZ样品的小 ;从阻抗谱图上可以看出 ,随着Al2 O3含量的增加 ,晶界电阻不断减小 ,在掺杂比例为 4 % (质量分数 )时 ,达到最小点。而后随着Al2 O3含量的增加 ,晶界电阻又呈上升趋势。用纯YSZ和掺 4 % (质量分数 )Al2 O3的材料制成SOFC ,得到伏安特性曲线 ,结果表明 ,掺 4 % (质量分数 )Al2 O3的性能比YSZ好。     

板状C/C复合膜的制备及其气体分离性能

以商用PMDA-ODA型聚酰胺酸为涂膜液,采取旋转涂膜技术在煤基板状炭膜支撑体上制备成C/C复合膜.研究了旋转涂膜次数、支撑体性质、支撑体表面预浸渍处理及加入表面改性剂对C/C复合膜气体分离性能的影响,采用扫描电镜对炭膜的复合效果和微结构进行表征.结果表明:随着旋转涂膜次数的增加,气体的渗透速率下降、分离系数增加;与无烟煤支撑体相比,以烟煤支撑体制备的C/C复合膜气体渗透速率和分离系数均较大;无烟煤支撑体经预浸渍处理后可以提高C/C复合膜的气体渗透速率;涂膜液中加入表面改性剂可以改善涂膜液和支撑体的复合效果,经一次涂膜即可制备出具有分子筛分性质的C/C复合膜.以烟煤为支撑体制备的C/C复合膜对H2/N2、CO2/N2和O2/N2的分离系数分别为94.3、18.3和10.2;空气中O2/N2分离系数为10.8,氧气的渗透速率为4.99×10-9 mol·m-2· s-1· pa-1,一次富集氧气浓度达到74.4％.     

Effect of Previous Milling of Precursors on Magnetoelectric Effect in Multiferroic {\mathrm{Bi}_{5}\mathrm{Ti}_{3}\mathrm{FeO}_{15}} Ceramic

$\mathrm{Bi}_{5}\mathrm{Ti}_{3}\mathrm{FeO}_{15}$ Bi 5 Ti 3 FeO 15 magnetoelectric (ME) ceramics have been synthesized and investigated. The ME effect can be described as an induced electric polarization under an external magnetic field or an induced magnetization under an external electric field. The materials in the ME effect are called ME materials, and they are considered to be a kind of new promising materials for sensors, processors, actuators, and memory systems. Multiferroics, the materials in which both ferromagnetism and ferroelectricity can coexist, are the prospective candidates which can potentially host the gigantic ME effect. $\mathrm{Bi}_{5}\mathrm{Ti}_{3}\mathrm{FeO}_{15}$ Bi 5 Ti 3 FeO 15 , an Aurivillius compound, was synthesized by sintering a mixture of $\mathrm{Bi}_{2}\mathrm{O}_{3}, \mathrm{Fe}_{2}\mathrm{O}_{3}$ Bi 2 O 3 , Fe 2 O 3 , and $\mathrm{TiO}_{2}$ TiO 2 oxides. The precursor materials were prepared in a high-energy attritorial mill for (1, 5, and 10) h. The orthorhombic $\mathrm{Bi}_{5}\mathrm{Ti}_{3}\mathrm{FeO}_{15}$ Bi 5 Ti 3 FeO 15 ceramics were obtained by a solid-state reaction process at 1313 K. The ME voltage coefficient ( $\alpha _\mathrm{ME}$ α ME ) was measured using the dynamic lock-in method. The highest ME voltage coefficient ( $\alpha _\mathrm{ME} = 8.28\,\text{ mV }{\cdot }\text{ cm }^{-1}{\cdot }\text{ Oe }^{-1})$ α ME = 8.28 mV · cm ? 1 · Oe ? 1 ) is obtained for the sample milled for 1 h at $H_\mathrm{DC }= 4$ H DC = 4  Oe (1 Oe = 79.58  $\text{ A }{\cdot }\text{ m }^{-1})$ A · m ? 1 ) .     

La0.67-xCa0.33MnO3系列样品的磁热效应

用溶胶-凝胶法制备了不同空位浓度掺杂的La0.67-xCa0.33MnO3系列样品(x=0.00,0.02,0.06,0.10),用扫描电子显微镜(SEM)观察了样品的形态和颗粒大小,X射线衍射实验结果显示样品为单相钙钛矿结构,用振动样品磁强计(VSM)测量了样品的磁化强度随温度变化的M-T曲线和起始磁化M-H曲线.研究了空位浓度对样品的居里温度Tc和磁熵变的影响.结果表明,空位浓度的掺杂将样品的居里温度Tc提高至室温附近,磁熵变得到增强.对于经历了一级相变的样品La0.67-xCa0 33MnO3(x=0.02),在居里温度Tc(277 K)附近和1T外磁场下,最大磁熵变达到了2.78 J/(kg·K).     

Dislocation structure at a \{ {\overline{1} 2\overline{1} 0} \}/ {\langle} 10\overline{1} 0 {\rangle} low-angle tilt grain boundary in LiNbO3

LiNbO₃ is a ferroelectric material with a rhombohedral R3c structure at room temperature. A LiNbO₃ bicrystal with a $ \{ {\overline{1} 2\overline{1} 0} \}/ {\langle}10\overline{1} 0{\rangle}$ 1° low-angle tilt grain boundary was successfully fabricated by diffusion bonding. The resultant boundary was then investigated using high-resolution TEM. The boundary composed a periodic array of dislocations with $ b = { 1}/ 3{\langle} \overline{1} 2\overline{1} 0{\rangle} $ . They dissociated into two partial dislocations by climb. A crystallographic consideration suggests that the Burgers vectors of the partial dislocations should be $ 1/ 3{\langle}01\overline{1} 0{\rangle} $ and $ 1/ 3{\langle}\overline{1} 100{\rangle} $ , and a stacking fault on $ \{ {\overline{1} 2\overline{1} 0} \} $ is formed between the two partial dislocations. From the separation distance of a partial dislocation pair, a stacking fault energy on $ \{ {\overline{1} 2\overline{1} 0} \} $ was estimated to be 0.25?J/m² on the basis of isotropic elasticity theory.     

LY12铝合金微弧氧化陶瓷层的结构和性能

分析了LY12铝合金微弧氧化陶瓷膜的形貌、组成和结构,研究了氧化膜的硬度、与基体的结合强度以及在油润滑和干摩擦这两种条件下的摩擦学行为.结果表明,铝合金微弧氧化膜可分为疏松层和致密层,疏松层由α-Al2O3、γ-Al2O3以及Al-Si-O相组成,致密层由α-Al2O3和γ-Al2O3组成,致密层中α-Al2O3的含量远远高于疏松层.从表层到基体,微弧氧化膜的断面显微硬度先增大后减 小.微弧氧化膜与铝合金基体结合紧密.随着膜厚度的增加,氧化膜的临界载荷线性增加.氧化膜具有优良的抗磨性能,油润滑条件下的摩擦系数仅为干摩擦下的1/10.     

Distribution of relaxation times investigation of $$\hbox {Co}^{3+}$$ doping lithium-rich cathode material $$\hbox {Li}[\hbox {Li}_{0.2} \hbox {Ni}_{0.1} \hbox {Mn}_{0.5} \hbox {Co}_{0.2}]\hbox {O}_{2}$$Li[Li0.2Ni0.1Mn0.5Co0.2]O2

The element \(\hbox {Co}^{3+}\) was introduced into lithium-rich material \(0.5\hbox {Li}_{2}\hbox {MnO}_{3} \cdot 0.5 \hbox {LiNi}_{0.5}\hbox {Mn}_{0.5}\hbox {O}_{2}\) by a polyacrylamide-assisted sol–gel method to form \(\hbox {Li}[\hbox {Li}_{0.2} \hbox {Ni}_{0.1} \hbox {Mn}_{0.5} \hbox {Co}_{0.2}]\hbox {O}_{2}\) and better electro-chemical performances were observed. Electrochemical impedance spectroscopy spectra were measured on 11 specific open circuit voltage levels on the initial charge profile. Then they were converted to the distribution of relaxation times (DRTs) g(\(\tau \)) by self-consistent Tikhonov regularization method. The obtained DRTs offered a higher resolution in the frequency domain and provided the number and the physical origins of loss processes clearly. Through the analysis of DRTs, the rapid augmentation of resistance to electronic conduction and charge transfer within the voltage range 4.46–4.7 V where the removal of \(\hbox {Li}_{2}\hbox {O}\) from \(\hbox {Li}_{2} \hbox {MnO}_{3}\) component took place was the most remarkable phenomenon and the \(\hbox {Co}^{3+}\) doping greatly reduced the resistance to electronic conduction Re. This gave us more evidence about the complicated ‘structurally integrated’ composite character of the material.     

\text{ CO}_{2} Laser-Based Pulsed Photoacoustic Ammonia Detection

Detecting ammonia traces is relevant in health, manufacturing, and security areas, among others. As ammonia presents a strong absorption band (the $\nu _{2}$ mode) around 10  $\upmu $ m, some of the physical properties which may influence its detection by means of pulsed photoacoustic (PA) spectroscopy with a TEA $\text{ CO}_{2}$ laser have been studied. The characteristics of the ammonia molecule and the laser intensity may result in a nonlinear dependence of the PA signal amplitude on the laser fluence. Ammonia absorption can be described as a simple two-level system with power broadening. As $\text{ NH}_{3}$ is a polar molecule, it strongly undergoes adsorption phenomena in contact with different surfaces. Therefore, physical adsorption–desorption at the cell’s wall is studied. A theoretical model, based on Langmuir’s assumptions, fits well to the experimental results with stainless steel. Related to these studies, measurements led to the conclusion that, at the used fluenced values, dissociation by multiphotonic absorption at the 10P(32) laser line may be discarded. A calibration of the system was performed, and a detection limit around 190 ppb (at 224 $\text{ mJ}\cdot \text{ cm}^{-2}$ ) was achieved.     

Evidence for One-Gap Superconductivity in Mg(B_{1-x}C_{x})_{2} Single Crystals at x=0.132 by Point-Contact Spectroscopy

We report the results of directional point-contact measurements in Mg(B $_{1-x}$ C $_{x})_{2}$ single crystals. The amplitudes of the gaps, $\Delta_{\pi}$ and $\Delta_{\sigma}$ , were determined for each C content by fitting the experimental low-temperature normalized conductance curves of our “soft” point contacts with the BTK model generalized to the two-band case. We found that, on increasing the carbon content, $\Delta_{\sigma}$ decreases almost linearly with $T_{c}$ and $\Delta_{\pi}$ slightly increases until, at $x=0.132$ (where $T_{c}=19$ K), they assume the same value $\Delta =3.2 \pm 0.9$ meV. This result is confirmed by the temperature and magnetic-field dependence of the conductance curves at this C content, which do not show any evidence of two distinct gap values. In particular, the Δ versus T curve follows very well a standard BCS curve, with a gap ratio $2\Delta /k_{B} T_{c}=3.9$ . These experimental findings are compared to the theoretical predictions of the two-band model in the Eliashberg formulation.     

Molecular beam epitaxy of semipolar AlN(11\bar{2}2) and GaN(11\bar{2}2) on m-sapphire

We report on the plasma-assisted molecular-beam epitaxy of semipolar $\hbox{AlN}(11\bar{2}2)$ and GaN( $11\bar{2}2$ ) films on $(1\bar{1}00)$ m-plane sapphire. AlN deposited on m-sapphire settles into two main crystalline orientation domains, $\hbox{AlN}(11\bar{2}2)$ and $\hbox{AlN}(10\bar{1}0),$ whose ratio depends on the III/V ratio. Growth under moderate nitrogen-rich conditions enables to isolate the $(11\bar{2}2)$ orientation. The in-plane epitaxial relationships of $\hbox{AlN}(11\bar{2}2)$ on m-plane sapphire are $[11\bar{2}\bar{3}]_{\rm AlN} \vert \vert [0001]_{\rm sapphire}$ and $[1\bar{1}00]_{\rm AlN} \vert \vert [11\bar{2}0]_{\rm sapphire}.$ GaN deposited directly on m-sapphire results in ( $11\bar{2}2$ )-oriented layers with ( $10\bar{1}\bar{3}$ )-oriented inclusions. A ～100 nm-thick AlN( $11\bar{2}2$ ) buffer imposes the ( $11\bar{2}2$ )-orientation for the GaN layer grown on top. By studying the Ga-desorption on GaN( $11\bar{2}2$ ), we conclude that these optimal growth conditions corresponds to a Ga excess of one monolayer on the GaN( $11\bar{2}2$ ) surface.     

Ga doping induced structural and optical modification in $$\hbox {Ge}_{2}\hbox {Sb}_{2}\hbox {Te}_{5}$$ Ge 2 Sb 2 Te 5 thin films

\(\text {Ge}_2\text {Sb}_2\text {Te}_5\) (GST) is considered a promising candidate for next-generation data storage devices due to its unique property of non-volatility and low power consumption. In present work, the bulk alloys and thin films of (\(\text {Ge}_2\text {Sb}_2\text {Te}_5\))\(_{100-x}\text {Ga}_x\) (x = 0, 3, and 10) are prepared using melt quenching and thermal deposition method, respectively. The effect of Ga doping on host composition is investigated by analyzing X-ray diffraction patterns and field emission scanning electron microscope images. From obtained results, it is found that all doped thin films retained the amorphous nature and exhibited uniform and smooth morphology. In Raman spectra, the appearance of a new peak in 10% Ga-doped GST thin film indicated an alteration in the atomic arrangement of host lattice. Transmission spectra revealed the highly transparent nature of all deposited thin films in the near-infrared region. The optical band gap of Ga-doped GST thin film is lower than that of the pure GST thin film which can be correlated with an increase in band tailing, attributed to an increase in localized defect states in the band gap. Due to the pronounced electronegativity difference between the Ga and Te element, new Ga–Te bonds with a higher number of wrong bonds (Ge–Ge, Sb–Sb, and Ge–Sb) are expected to thermally stabilize the amorphous phase. Such results predict the better performance of Ga-doped GST composition for better performance of phase-change random access memory.

     

Study of Structural Modification and Fluctuation Induced Electrical Conductivity in \text {YBa}_{2}\text {Cu}_{3}\text {O}_{7-y}+x \text {BaSnO}_{3} Superconductor Composite

A series of \((1-x) \text {YBa}_{2}\text {Cu}_{3}\text {O}_{7-y} + x \text {BaSnO}_{3 }(x = 0.0, 0.1, 0.3, 0.5, 1.0, 2.5, 5.0\,\text {wt}{\%})\) samples were prepared using the solid-state reaction method. XRD graphs confirm the orthorhombic structure in pristine as well as in composite samples. Raman spectra show the presence of all the vibration modes in pure as well as in the composite samples. In addition, some defect-induced modes have also appeared in the higher weight % BSO-added sample, and no loss of apical oxygen O(4) at 500 cm \(^{-1}\) occurs due to BaSnO \(_{3}\) (BSO) addition. Microstructural analysis reveals the unchanged grain size with the incorporation of dielectric BSO particles in the YBCO matrix. Superconducting transition temperature determined from standard four-probe method decreases with the increase of BSO wt%. Excess conductivity fluctuation analysis using Aslamazov–Larkin model fitting reveals transition of two dominant regions (2D and 3D) above \(T_\mathrm{c}\) . 2D to 3D crossover temperature i.e. Lawrence–Doniach temperature that demarcates dimensional nature of fluctuation inside the grains is influenced by BSO incorporation in YBCO matrix.