溶胶-凝胶固相微萃取涂层及其在农药残留分析中的应用

利用溶胶-凝胶(sol-gel)技术制备固相微萃取(SPME)涂层材料.通过硅醇盐前驱体与涂层聚合物羟基硅油(OH-TSO)的水解共聚的方法,成功地制备了聚二甲基硅氧烷sol-gel 涂层的SPME 萃取头,并以农药的混合标准水溶液为研究对象,用直接-固相微萃取-气相色谱法(GC)对涂层的性能进行考察,制成的萃取头适用于多种农药残留的萃取分离分析.     

Sol-gel bioactive glass-ceramics Part II: Glass-ceramics in the CaO-SiO2-P2O5-MgO system

Ceramics, with basic composition based on the CaO-SiO₂-P₂O₅-MgO system with different Ca+ Mg/P+Si molar ratio (R), were prepared via polystep sol-gel technique. The structure of the obtained ceramic materials has been studied by XRD, FTIR spectroscopy, and SEM. X-ray diffraction showed the presence of akermanite and HA for the sample with R = 1.68 and Mg substituted β-TCP and silicocarnotite for the sample with R = 2.16, after thermal treatment at 1200°C/2 h. The obtained results are in good agreement with FTIR. In vitro test for bioactivity in static condition proved that the carbonate containing hydroxyapatite (CO₃HA) can be formed on the surface of the synthesized samples. CO₃HA consisted of both A- and B-type CO₃²⁻ ions. SEM micrographs depicted different forms of HA particles, precipitated on the surface after soaking in 1.5 simulated body fluid (SBF).      

溶胶-凝胶法原位生成SiO2改性硅基耐烧蚀材料

建立了在硅基耐烧蚀材料中用溶胶-凝胶法原位生成SiO2的方法.首先将硅橡胶、气相白炭黑、纤维等原料混炼硫化制备出硫化胶.然后将硫化胶依次浸入四氢呋喃、原硅酸乙酯和正丁基胺水溶液中进行预溶胀处理、物理扩散和化学反应,得到原位生成SiO2.SEM照片显示,在硅基耐烧蚀材料中原位生成的SiO2颗粒呈球形,粒径在40~60 nm,但分布不均匀,在硫化胶表层存在富集现象.实验结果表明,原位生成SiO2平均含量增加,硅基耐烧蚀材料的抗拉强度增加,线烧蚀率下降;含13.7%原位生成SiO2硅基耐烧蚀材料抗拉强度为5.82 MPa,线烧蚀率为0.071 mm/s.     

TiO_2/SiO_2纳米薄膜的光催化活性和亲水性

通过 sol-gel工艺在钠钙玻璃表面制备了均匀透明的 TiO2/SiO2复合纳米薄膜 .实验结果表明 : 当 SiO2添加量较高时 , TiO2/SiO2复合纳米薄膜的光催化活性明显降低 ;当 SiO2添加量较低时 ,TiO2/SiO2复合薄膜的光催化活性无明显变化 .在 TiO2薄膜中添加 SiO2,可以抑制薄膜中 TiO2晶粒的长大 ,同时薄膜表面的羟基含量增加 , 水在复合薄膜表面的润湿角下降 , 亲水能力增强 .当 SiO2含量为 10％－ 20％（摩尔分数）时获得了润湿角为 0°的超亲水性薄膜 .     

溶剂热法制备Ag/TiO2纳米材料及其光催化性能

以乙醇为溶剂, 钛酸四丁酯为前驱体, 用溶剂热法制备了Ag表面修饰的负载型纳米二氧化钛光催化剂. 利用X射线衍射(XRD)、N₂吸附-脱附(BET)、透射电子显微镜(TEM)、X射线光电子能谱(XPS)、紫外-可见(UV-Vis)光谱等技术对其进行了系统的表征, 以亚甲基蓝(MB)溶液的脱色降解为模型反应, 考察了不同Ag含量样品的光催化性能. 结果表明: 用溶剂热法制备的样品中TiO₂皆为锐钛矿相, 金属Ag颗粒沉积在TiO₂表面, 粒径为2 nm左右, 比表面积较溶胶凝胶法制备的样品大大增加, 最高可达151.44 m²·g^-1; UV-Vis光谱和光催化实验表明: Ag修饰使TiO₂对光的吸收能力大大增强, 吸收带边红移至可见光区, 亚甲基蓝在该复合材料上的光催化降解反应遵循一级反应动力学模型; 溶剂热法制备样品的光催化性能明显好于溶胶凝胶法制备的样品, 在紫外光和可见光下, Ag摩尔分数为5%的样品表现出最佳的光催化活性.     

溶剂热法制备Ag/TiO2纳米材料及其光催化性能

以乙醇为溶剂, 钛酸四丁酯为前驱体, 用溶剂热法制备了Ag表面修饰的负载型纳米二氧化钛光催化剂. 利用X射线衍射(XRD)、N₂吸附-脱附(BET)、透射电子显微镜(TEM)、X射线光电子能谱(XPS)、紫外-可见(UV-Vis)光谱等技术对其进行了系统的表征, 以亚甲基蓝(MB)溶液的脱色降解为模型反应, 考察了不同Ag含量样品的光催化性能. 结果表明: 用溶剂热法制备的样品中TiO₂皆为锐钛矿相, 金属Ag颗粒沉积在TiO₂表面, 粒径为2 nm左右, 比表面积较溶胶凝胶法制备的样品大大增加, 最高可达151.44 m²·g^-1; UV-Vis光谱和光催化实验表明: Ag修饰使TiO₂对光的吸收能力大大增强, 吸收带边红移至可见光区, 亚甲基蓝在该复合材料上的光催化降解反应遵循一级反应动力学模型; 溶剂热法制备样品的光催化性能明显好于溶胶凝胶法制备的样品, 在紫外光和可见光下, Ag摩尔分数为5%的样品表现出最佳的光催化活性.     

溶剂热法制备Ag/TiO2纳米材料及其光催化性能

以乙醇为溶剂, 钛酸四丁酯为前驱体, 用溶剂热法制备了Ag表面修饰的负载型纳米二氧化钛光催化剂. 利用X射线衍射(XRD)、N₂吸附-脱附(BET)、透射电子显微镜(TEM)、X射线光电子能谱(XPS)、紫外-可见(UV-Vis)光谱等技术对其进行了系统的表征, 以亚甲基蓝(MB)溶液的脱色降解为模型反应, 考察了不同Ag含量样品的光催化性能. 结果表明: 用溶剂热法制备的样品中TiO₂皆为锐钛矿相, 金属Ag颗粒沉积在TiO₂表面, 粒径为2 nm左右, 比表面积较溶胶凝胶法制备的样品大大增加, 最高可达151.44 m²·g^-1; UV-Vis光谱和光催化实验表明: Ag修饰使TiO₂对光的吸收能力大大增强, 吸收带边红移至可见光区, 亚甲基蓝在该复合材料上的光催化降解反应遵循一级反应动力学模型; 溶剂热法制备样品的光催化性能明显好于溶胶凝胶法制备的样品, 在紫外光和可见光下, Ag摩尔分数为5%的样品表现出最佳的光催化活性.     

Effect of metal ions on structural,morphological and optical properties of nano-crystallite spinel cobalt-aluminate (CoAl2O4)

The bright blue nano crystallite cobalt aluminate (CoAl₂O₄) was synthesized by sol–gel method using a mixture of chelating agent of glycerol and citric acid. The effects of changing (0.05, 0.075, 0.10, 0.25, 0.50, and 0.75 mol/L) metal ion concentration on the structural, morphological and color properties of synthesized CoAl₂O₄ were characterized by using X-ray diffraction (XRD), Scanning electron microscopy (SEM), Energy dispersive X-ray spectroscopy (EDX), Fourier transform infrared spectroscopy (FTIR), Nanoparticle size analyzer, Simultaneous Thermal Analyzer (STA), UV–vis absorption spectroscopy, and CIE-LAB colorimetric analysis. From the X-ray peak profile analysis, the crystallite size was measured by Debye-Scherrer (D-S) equation, and three different models presenting average crystallite sizes between 88.3 and 125.4 nm.The average lattice strain, dislocation density, lattice constant, cell volume, and zeta potential were between 0.00021 and 0.0058, (1.73 to 12.8) × 10¹⁴ (lines/m²), 8.10658 to 8.11181 Å, 533.60 to 533.81 Å³, ?56.4 to ? 63.5 mV, respectively. Using UV–vis absorption spectroscopy, the band gap was calculated from Kubelka-Munk method, and the values of band gap increasing from 1.82 to 1.84 eV, respectively. The reflectance spectra and the CIE-L*a*b* values of cobalt aluminate is also measured which confirmed the formation of blue nano crystallite cobalt aluminate.     

常压干燥法制备气凝胶的研究进展

气凝胶是一类轻质、低密度的三维纳米多孔固态材料,因其独特的高孔隙率、高比表面积和低导热系数等特性,使其在吸附、催化、保温隔热和隔音等诸多领域具有广泛的用途,目前其相关研究在材料科学领域受到了广泛的关注。气凝胶的制备主要包括溶胶-凝胶过程和湿凝胶干燥两个步骤,湿凝胶的干燥是制备气凝胶过程中至关重要而又较为困难的一步。传统的气凝胶通过超临界干燥制备,工艺复杂、成本高,而且由于干燥过程在高温高压条件下进行,有一定的危险性并且不适宜大规模生产,因此如何通过常压干燥获得高比表面积、高孔隙率、低密度的性能优异的气凝胶是其研究的重要方向之一。本文简要介绍了湿凝胶的制备以及凝胶干燥理论,详细介绍了近年来常压干燥方法气凝胶制备的研究进展,并对其未来发展前景做出了展望。     

Amino-Acid-Induced Circular Polarized Luminescence in One-Dimensional Manganese(II) Halide Hybrid

Circular polarized luminescence (CPL)-active materials attract great attentions owing to their widely applications in 3D optical displays and encrypted transmission. Inspired by the strategies adopted in perovskite based CPL materials, herein, CPL-active hybrids (D)- and (L)-(tert-butyl prolinate)MnCl₃ were successfully prepared by assembling chiral D/L tert-butyl prolinate with manganese (II) chloride. Single crystal structures show the as-formed hybrids possess one-dimensional (1D) structure containing linear chains of face-sharing MnCl₆ octahedral surrounded by prolinate cations. The 1D Mn(II) hybrids display strong red emission peaked at 646 nm with PLQY of 67.1 % and 57.2 % for d -type and l -type, respectively, representing the highest PLQY for 1D Mn^II hybrids. Interestingly, the 1D Mn(II) hybrids exhibit prominent circular dichroism (CD) signals and remarkable CPL activity with the dissymmetry factor g of 6.1*10⁻³ and −6.3*10⁻³ from 550 to 800 nm for (D)- and (L)-(tert-butyl prolinate)MnCl₃, respectively, owing to the existence of chiral cations. It is worthy noted the obtained g represents the highest value for non-lead organic–inorganic hybrids.