Pechini溶胶-凝胶法制备SiO2/TiO2复合微粒

采用超声St(o)ber法制备了单分散性的纳米载体SiO2,再采用Pechini溶胶-凝胶制备法制备出SiO2/TiO2复合微球.通过X射线衍射仪、场发射扫描电子显微镜(FESEM)对粉体的晶型和显微形貌进行测试分析.结果表明:纳米载体SiO2球形颗粒为无定形态,Ti02粉体为形貌多样的块状颗粒,大颗粒粒径大于10μm...     

溶胶-凝胶法制备YBa2Cu3O7-x超导薄膜的研究

传统的TFA-MOD法制备YBa2Cu3O7-x薄膜,采用Y、Ba、Cu 3种金属的三氟醋酸盐(TFA)为先驱体,在热分解时,会产生大量的HF气体,即使通过将近20h的缓慢升温过程来对薄膜进行热分解,也难以获得较为光洁的表面,从而无法实现厚膜的制备.本文提出了一种新的含氟溶胶-凝胶工艺,通过减少溶胶中F的含量,并利用二乙醇胺做修饰剂,缩短了热分解时间,提高了薄膜的表面光洁度.利用该方法在(010)LaAlO3衬底上制备了具有良好c轴取向,临界转变温度为89K的YBCO超导薄膜.     

Effective thermal conductivity of Cu/diamond composites containing connected particles

An analytical model for the thermal conductivity of Cu/diamond composites with connected particles is presented by replacement of a cluster of connected particles with an equivalent polycrystal subsequently using a multiple effective medium approach. By applying this model to the measured thermal conductivity of Cu/diamond composites prepared by high pressure high temperature sintering technique reported in the literature, we show that it quite well describes the observed thermal conductivity enhancement induced by the connected particles. We estimate the value of connected particle loading in real composites and show that large particles are easier to form the bonding contact than small particles. The present work also demonstrates that the sensitivity of thermal conductivity contribution from the connected particles strongly depends on the particle size, and their pronounced thermal conductivity enhancement should lie within the certain particle size range.     

石墨表面化学镀Cu对天然鳞片石墨/Al复合材料热物理性能的影响

对天然鳞片石墨（GF）进行化学镀Cu的表面处理,对化学镀Cu石墨（Cu-GF）和Al粉采用真空热压的工艺制备出镀Cu石墨/Al（Cu-GF/Al）复合材料。研究了Cu-GF/Al复合材料的微观结构和微观界面,同时也研究了Cu-GF对Cu-GF/Al复合材料热导率和抗弯性能的影响。结果表明,GF上的Cu层能抑制界面脆弱相Al₄C₃的产生,使Cu-GF/Al复合材料的抗弯性能有了显著提升。当Cu-GF体积分数从50%增加到70%时,Cu-GF/Al复合材料的抗弯强度也从104 MPa降低到74 MPa。当GF体积分数为70%时,Cu-GF/Al复合材料的热导率达到最高值为522 W/（m·K）。     

Phase development and activation energy of the Y2O3-Al2O3 system by a modified sol-gel process

The phase development of Y₃Al₅O₁₂ (YAG), YAlO₃ (YAP), and Y₄Al₂O₉ (YAM) synthesized by a modified sol-gel method has been studied. A chelate agent (ethyl acetoacetate) is added to control the hydrolysis and to modify the sol-gel process. The sol-gel-derived powder is then heat-treated to induce crystallization. The X-ray diffraction method is employed to determine the crystalline phases of the resulting powders. The formation of YAG, YAP, and YAM is described. For both YAP and YAM compositions, there is a phase transformation from YAP polymorphism to perovskite YAP. The activation energies of YAG are estimated at about 69 kcal/mol by the isothermal process as fitted with the Johnson-Mehl-Avrami equation and about 222 ± 2 kcal/mol by the continuous heating method as fitted with Kissinger and Sotgiu plots. The difference of activation energies calculated from the two methods is mainly due to the complicated crystallization of YAG.     

溶胶-凝胶法制备聚酰亚胺/Al2O3纳米复合材料的研究

采用溶胶-凝胶法制备了聚酰亚胺(PI)/Al2O3纳米复合薄膜,通过测定胶液在贮存过程中粘度的变化研究了纳米复合胶液的贮存稳定性,采用热失重分析、拉伸强度和体积电阻率等测试方法研究了纳米复合薄膜的性能.结果表明,当Al2O3含量不大于14%时,纳米Al2O3前驱体的存在对纳米复合胶液的贮存稳定性影响不大或基本上没有影响;与纯PI薄膜相比,Al2O3含量不大于5%时,纳米复合薄膜的表观分解温度、拉伸强度以及常态下的体积电阻率均有明显提高;纳米Al2O3的存在有利于改善薄膜的高温电性能.     

Superconducting properties of the lithium-substituted YBa2Cu4O8 prepared by the sol-gel method

The effects of the lithium substitution for copper on the properties of the superconducting YBa₂Cu₄O₈ were studied. Single-phase YBa₂Cu_4–x LixO₈ was successfully prepared by the sol-gel method under ambient pressure over a composition range of 0x 0.08, while impurity phases appeared at x=0.10 and 0.20. The lattice constants of YBa₂Cu_4–x Li _x O₈ were almost invariant with increasing lithium content x. The superconducting transition temperature decreased monotonically with increasing x in the range, 0x0.08. The suppression of superconductivity was discussed in terms of the impurity effect in the CuO₂ planes.     

An investigation on electroless Cu–P composite coatings with micro and nano-SiC particles

Cu–P/micro-SiC and Cu–P/nano-SiC composite coatings were deposited by electroless plating and their composition and microstructure were observed by EDX (energy-dispersive analysis), SEM (scanning electron microscope) and XRD (X-ray diffraction). The corrosion resistance, microhardness and the wear resistance of the Cu–P/nano-SiC composite coatings were measured and the comparison with those of Cu coatings and Cu–P/micro-SiC coatings were given. The anti-corrosion properties of Cu coatings were investigated in 3.5% NaCl solution by the potentiodynamic polarisation and electrochemical impedance spectroscopy (EIS) techniques. Among three kinds of Cu–P based coatings, the corrosion resistance, hardness and wear resistance of Cu–P/nano-SiC coatings were the largest. This indicates that the precipitation of nano-SiC particles would improve the corrosion resistance, hardness and wear resistance of the Cu–P coatings significantly.     

亚砜基纤维素膜制备及SO2渗透机理研究

采用苯基乙烯基亚砜对纤维素膜进行化学改性，制备了亚砜基纤维素膜，并测试了其SO2气体渗透性能；观察到该膜对SO2的渗透系数随气体压力增大而减小，符合双吸附一双迁移模型．     

Fabrication of silica/platinum core-shell particles by electroless metal plating

An electroless metal plating method was used to form Pt shells on sub-micrometer-sized silica (SiO₂) particles fabricated by a sol-gel method. The electroless metal plating method was comprised of three steps: (1) surface-modification of SiO₂ particles with polyvinylpyrrolidone (PVP) (SiO₂/PVP) or poly-diallyldimethylammonium chloride (PDADMAC) (SiO₂/PDADMAC), (2) pre-deposition of Pt nuclei or Pt fine particles on the SiO₂ particles by reducing Pt ions in the presence of SiO₂/PVP particles (SiO₂/PVP-Pt) or SiO₂/PDADMAC particles (SiO₂/PDADMAC-Pt), and (3) growth of the pre-deposited Pt by immersing the SiO₂/PVP-Pt or SiO₂/PDADMAC-Pt particles in a Pt-plating solution. The pre-deposition of Pt nanoparticles was successfully performed for the surface-modified SiO₂ particles since the surface modification possibly strengthened the affinity between the SiO₂ particle surfaces and Pt ions. The Pt nanoparticles were pre-deposited more uniformly in the case of PVP because the pre-deposition took place more slowly for the PVP, which provided uniform surface-modification followed by the uniform pre-deposition of Pt nanoparticles. The formation of Pt shells was successfully performed on the SiO₂/PVP-Pt particles in the electroless metal plating process because Pt nuclei were generated by the reduction of H₂PtCl₆ and then further deposited on the Pt particle surfaces on the SiO₂/PVP-Pt particles.     

Energy gap symmetry and thermal conductivity of YBa2Cu3O7

The characteristic enhancement in the heat conduction below T_c is analyzed on sintered YBa₂Cu₃O₇ from viewpoints of both d-wave and s-wave coupling. Assuming the existence of a large energy gap Δ₀(≥1.5Δ _BCS ), only d-wave coupling is consistent with experimental observation. It is found that the most reasonable explanation for the enhancement is provided by the weak-coupling phonon conduction model under d-wave energy gap.     

异丙醇铝溶胶-凝胶掺杂的SiO2-Al2O3/PEG导热增强型定形相变储能材料

以异丙醇铝(AIP)与正硅酸乙酯(TEOS)为溶胶前驱体、聚乙二醇(PEG)为相变组分,经超声辅助溶胶-凝胶过程制备了SiO2-Al2O3/PEG导热增强型定形相变储能材料.利用FTIR和XRD对SiO2-Al2O3/PEG进行结构表征及结晶性能测定,利用DSC与TGA研究其热性能与热稳定性,利用显微热台与数码拍照技术测试材料的定形效果;利用热导率仪测定了材料的导热系数.结果表明,SiO2-Al2O3/PEG的相变焓值可以达到100 J/g以上,低于300℃时具有良好的热稳定性,当SiO2-Al2O3/PEG中的铝硅质量比为0.2∶1时,其导热系数可达0.414 W/(m·K),导热性能比纯PEG提高39.3％,并具有良好的定形效果.     

Single-crystal growth and characterization of Cu2O and CuO

We have prepared a large number of crystals of cuprous oxide (Cu2O) by various procedures. Photoluminescence spectra of these crystals were studied to examine the concentration of defects, especially copper vacancy VCu to seek favourable conditions for growing Cu2O crystal. High-quality single crystals of Cu2O were prepared by the floating-zone melting method in air. Several synthetic crystals (specimens FA, FZ and GZ) and also a natural crystal were studied by X-ray analysis, inductively coupled plasma spectroscopy analysis, optical absorption, photoluminescence, photoconductivity and cyclotron resonance absorption, photoluminescence, photoconductivity and cyclotron resonance absorption to characterize their optical and electrical qualities. The best values of mobility and scattering time of photocarriers at T = 4.2 K are estimated to be h1.8 × 105 cm2 V–1 s–1 and h60 ps for positive holes, and 1.3 × 105 cm2 V–1 s–1 and 70 ps for electrons in Cu2O. Further, we report preliminary experimental results on transport property of crystals also of cupric oxide (CuO) purified by the floating-zone melting method.     

Enhanced photocatalytic performance of Cu2O nano-photocatalyst powder modified by ball milling and ZnO

In this paper, a ball milled Cu₂O-ZnO nano-photocatalyst with good photocatalytic performance in visible light range was prepared. Effect of ZnO presence and ball milling of Cu₂O on the structure, microstructure, optical properties and photocatalytic performance were studied. X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscope (TEM), high resolution transmission electron microscopy (HRTEM), diffuse reflectance spectroscopy (DRS), photoluminescence (PL) analysis and UV–Vis spectrophotometer were used as characterization techniques. FESEM results indicated that ball milling of Cu₂O changed the morphology of Cu₂O-ZnO composite. The uniform formation of ZnO particles with average size of 30 nm over the Cu₂O surface was observed. The formation of p-n heterostructure with good contact between Cu₂O and ZnO nanoparticles was found by HRTEM image. Ball milling of Cu₂O promotes visible light absorption and reduction band gap to 1.9 eV in Cu₂O-ZnO photocatalyst. Intensity of PL spectra for the ball milled Cu₂O-ZnO photocatalyst was obviously lower. Ball milled Cu₂O-ZnO photocatalyst shows the highest photocatalytic activity and degradation efficiency of 98% was obtained for 2 mg/L methylene blue (MB) solution after 240 min. The kinetics of the photodegradation was followed the Langmuir-Hinshelwood (L-H) model and degradation rates were decreased by increase of MB concentration. In the case of ball milled Cu₂O and presence of ZnO, the MB degradation kinetics was two times faster.     

Ionic conductivity and crystal structure relationships in Ti/Cu substituted Bi4V2O11

Crystal structure and oxide ion conductivity of a series of Ti and Ti-Cu double substituted Bi₄V₂O₁₁ compounds, Bi₂V_(1–x)Ti _x O_(11–x)/2 (0.085 x 0.15), and Bi₂V_0.9Cu_(0.1–x)TixO_5.35+x (0 x 0.1), were investigated using X-ray powder diffraction and ac impedance spectroscopy in the temperature and frequency range of 100–700°C and 10^–2–10⁷ Hz, respectively.Structural phase transitions, and , occur as a function of composition in Ti substituted compounds for which the is evidenced to be stable at room temperature when x exceeds 0.125. For all Ti-Cu double substituted compounds studied, the room temperature phase was identified to be phase.The required amount of Ti for phase stabilization at room temperature was significantly reduced and the conductivity improved when Cu substituted a part of Ti. Therefore, for the Bi₂V_0.9Cu_(0.1–x)Ti _x O_5.35+x (0 x 0.075) compounds the ionic conductivity increased and activation energy decreased with decreasing x. At low temperature, the highest ion conductivity was obtained for Bi₂V_0.9Cu_0.1O_5.35. At high temperature (T>500°C), a different behavior was observed. The total conductivity increased at first with decreasing x values down to x = 0.05 and then decreased. The maximum conductivity was obtained for Bi₂V_0.9Cu_0.05Ti_0.05O_5.4, and the activation energy decreased with decreasing x values, such as what happened at low temperature.