溶胶-凝胶法制备掺Er~(3+)玻璃及其光谱性质

本文描述了用溶胶－凝胶法制备掺Ｅｒ３＋的ＳｉＯ２干凝胶和玻璃，用差热分析（ＤＴＡ）和ＦＴＩＲ研究了干凝胶和玻璃的性质，测定了掺Ｅｒ３＋凝胶和玻璃的吸收光谱和荧光光谱。     

溶胶-凝胶法制备的GeO2-SiO2凝胶玻璃的红光发射

以3三氯锗丙酸和正硅酸乙酯为原料采用溶胶凝胶法制备了GeO2SiO2凝胶玻璃.室温下以532nm激光(Nd:YAG)激发GeO2SiO2凝胶玻璃有一强的发光峰,这种发光有两个发光带,其峰位分别在575nm和624nm.该发光现象是由镶嵌在GeO2SiO2凝胶玻璃中GeO2纳米颗粒产生的.利用吸收光谱和TEM对GeO2SiO2凝胶玻璃进行了表征,结果发现随着Ge含量的增加凝胶玻璃中GeO2纳米颗粒的尺寸越来越大,吸收边向低能边移动.X射线衍射和电子衍射确定GeO2SiO2凝胶玻璃中GeO2颗粒的结构为非晶结 关键词： GeO2-SiO2凝胶玻璃 溶胶-凝胶法 红光发射     

溶胶-凝胶法制备均相掺钛干凝胶

以溶胶-凝胶法制备掺钛干凝胶,采用冰乙酸控制钛酸四丁酯水解,结合钛源与硅源独立预水解技术制备前体掺钛溶胶和凝胶。考察了溶剂量、抑制剂量和掺钛量对溶胶稳定性和均匀性的影响,以及老化、干燥条件和掺钛量对凝胶均匀性的影响,并优化了工艺参数。结果表明,冰乙酸能够有效地控制钛源水解并改善溶胶均匀性,结合钛源和硅源独立预水解技术,能够可控地制备出掺钛溶胶。在乙醇与醇盐物质的量比为5、冰乙酸与钛酸四丁酯物质的量比为6、钛硅原子数比为2%~20%的条件下可以得到均匀、稳定的溶胶。钛硅原子数比低于10%的溶胶在100 ℃老化24 h,100 ℃开放条件下干燥24 h能够形成均匀的干凝胶。钛硅原子数比高于10%的凝胶在干燥过程中析出氯化钠,得不到均匀的凝胶。     

溶胶-凝胶法制备均相掺钛干凝胶

以溶胶-凝胶法制备掺钛干凝胶,采用冰乙酸控制钛酸四丁酯水解,结合钛源与硅源独立预水解技术制备前体掺钛溶胶和凝胶。考察了溶剂量、抑制剂量和掺钛量对溶胶稳定性和均匀性的影响,以及老化、干燥条件和掺钛量对凝胶均匀性的影响,并优化了工艺参数。结果表明,冰乙酸能够有效地控制钛源水解并改善溶胶均匀性,结合钛源和硅源独立预水解技术,能够可控地制备出掺钛溶胶。在乙醇与醇盐物质的量比为5、冰乙酸与钛酸四丁酯物质的量比为6、钛硅原子数比为2%~20%的条件下可以得到均匀、稳定的溶胶。钛硅原子数比低于10%的溶胶在100℃老化24h,100℃开放条件下干燥24h能够形成均匀的干凝胶。钛硅原子数比高于10%的凝胶在干燥过程中析出氯化钠,得不到均匀的凝胶。     

溶胶-凝胶法制备PbS量子点玻璃的研究

采用溶胶-凝胶法合成了半导体PbS量子点掺杂的Na₂O-B₂O₃-SiO₂玻璃,研究了不同热处理工艺对玻璃结构的影响,利用多种表征手段研究了量子点掺杂玻璃中的微晶结构及其光学性能.孔径分析结果表明随着热处理温度的升高玻璃内部孔径不断减小,最终孔结构几乎完全消失;红外光谱分析表明玻璃网络结构在较低温度下己经形成,随温度的升高不断密实化; X射线光电子能谱证明了玻璃中存在PbS,高分辨透射电镜表征了玻璃基质中掺杂的微晶结构是PbS,统计计算表明,玻璃中微晶的平均粒径尺寸为3.5nm;吸收光谱分析发现,微晶掺杂玻璃的吸收边界较PbS的块体材料发生了明显的蓝移,产生了量子尺寸效应;通过Z扫描技术测得其非线性折射率γ为-2.03×10^-14cm²/GW. 关键词： PbS量子点 半导体 非线性光学效应 溶胶-凝胶法     

铝对过渡金属离子掺杂的二氧化硅溶胶凝胶玻璃发光性质的影响

用溶胶凝胶法制备了过渡金属离子(Ni2+,Mn2+和Cu2+)单掺、铝共掺的二氧化硅玻璃,测量了荧光光谱、吸收光谱和红外光谱,研究了Al3+对过镀金属离子在二氧化硅玻璃中发光性质的影响。研究结果表明,Al3+对过渡金属离子的发光性质有着显著影响:Ni2+,Mn2+和Cu+的发光强度大幅度提高,Mn2+的发光峰峰位改变。     

块状TiO2气凝胶的溶胶-凝胶过程及结构

 对块状TiO₂气凝胶的溶胶-凝胶过程及结构进行了实验研究,结果发现：增加催化剂的量,凝胶化时间缩短,湿凝胶的透明度降低,强度提高;增加前驱体的量,凝胶化时间缩短,湿凝胶的透明度变化不大,强度提高;增加水量,凝胶化时间先缩短后增加,湿凝胶透明度先减小后增加,强度先增加后减小。利用扫描电镜对超临界干燥法制备的不同催化剂量和密度的块状TiO₂气凝胶的结构进行了表征,并对结构与溶胶-凝胶过程之间的联系进行了分析。结果表明：增加催化剂量,由于缩聚反应进行的程度提高,气凝胶粒子粒径较小且总的孔径较大。减小前驱体量,气凝胶粒子粒径增大且结构逐渐疏松。     

块状TiO2气凝胶的溶胶-凝胶过程及结构

对块状TiO2气凝胶的溶胶-凝胶过程及结构进行了实验研究,结果发现:增加催化剂的量,凝胶化时间缩短,湿凝胶的透明度降低,强度提高;增加前驱体的量,凝胶化时间缩短,湿凝胶的透明度变化不大,强度提高;增加水量,凝胶化时间先缩短后增加,湿凝胶透明度先减小后增加,强度先增加后减小。利用扫描电镜对超临界干燥法制备的不同催化剂量和密度的块状TiO2气凝胶的结构进行了表征,并对结构与溶胶-凝胶过程之间的联系进行了分析。结果表明:增加催化剂量,由于缩聚反应进行的程度提高,气凝胶粒子粒径较小且总的孔径较大。减小前驱体量,气凝胶粒子粒径增大且结构逐渐疏松。     

溶胶-凝胶法制备的光学薄膜表面粒度及其分布

本文研究了溶胶-凝胶法制备的光学薄膜表面粒度及其分布,结果表明:膜表面的粒度大小与热处理温度及陈化时间有关,粒度分布函数可分为泊松分布、正态分布等.     

平板波导的溶胶-凝胶法制备与测试

利用溶胶-凝胶法制作了平板波导.实验中,在不同的条件下采用溶胶-凝胶法在玻璃衬底上制备出TiO2平板波导,分析了影响平板波导的因素,如溶胶-凝胶溶液的浓度、pH值,滴胶速度,热处理等.并对在不同工艺条件下的波导膜特性进行了测试,分析了影响波导膜质量的各个因素.实验表明,在控制实验条件的前提下溶胶-凝胶法在制作平板波导膜的工艺上制作方法简单,容易实现.     

Effect of ZnO on phase emergence, microstructure and surface modifications of calcium phosphosilicate glass/glass-ceramics having iron oxide

The effect of ZnO on phase emergence and microstructure properties of glass and glass-ceramics with composition 25SiO₂-50CaO-15P₂O₅-(10 − x)Fe₂O₃-xZnO (where x = 0, 2, 5, 7 mol%) has been studied. They have been characterized using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and scanning electron microscopy (SEM). Surface modifications of these glass-ceramics in simulated body fluid have been studied using Fourier transform infrared reflection spectroscopy (FTIR), XPS and SEM. Results have shown a decrease in the fraction of non-bridging oxygen with increase in zinc oxide content. Emergence of crystalline phases in glass-ceramics at different heat treatment temperatures was studied using XRD. When glass is heat treated at 800 °C calcium phosphate, hematite and magnetite are developed as major phases in the glass-ceramics samples with ZnO up to 5 mol%. In addition to these, calcium silicate (Ca₃Si₂O₇) phase is also observed when glass is heat treated at 1000 °C. The microstructure of the glass-ceramics heat treated at 800 °C exhibits the formation of nano-size (40-50 nm) grains. On heat treatment at 1000 °C crystallites grow to above 50 nm size and more than one phase are observed in the microstructure. The formation of thin flake-like structure with coarse particles is observed at high zinc oxide concentration (x = 7 mol%). In vitro studies have shown the surface modifications and formation of Ca-P-rich layer on the glass-ceramics when immersed in simulated body fluids (SBF) for different durations. The bioactive response was found to depend on ZnO content.     

SiO2薄膜中咔唑的发光特性

利用溶胶-凝胶工艺制备了含咔唑的SiO2薄膜,实验测量了薄膜样品的光致发光特性.结果发现：样品不仅能发射红光,并且当激发波长从610 nm连续减小到400 nm时,其发射谱峰位又能从760 nm连续蓝移到550 nm左右.薄膜样品的荧光特性随激发波长而改变的现象可归因于咔唑分子被紧缩在凝胶内部的微孔中受到挤压而导致共轭尺寸发生变化.     

在NaCl和HTAB共存条件下甲基纤维素溶液凝胶化行为

利用流变仪研究了甲基纤维素(MC)溶液在NaCl、十六烷基三甲基溴化铵(HTAB)以及两者共存下MC溶液的凝胶化行为,发现其凝胶化温度随着NaCl浓度的增加而下降,随着HTAB浓度的增加而上升;但是MC/NaCl的凝胶化温度保持不变,与HTAB浓度 无关,而MC/HTAB溶液的凝胶化温度则随着NaCl浓度的增加而下降．以上的实验结果表明,在NaCl存在下,HTAB将被诱导形成胶束,因此MC/NaCl的凝胶化温度保持不变;反之,当NaCl不存在时,HTAB将优先吸附到MC上而不会在溶液中形成胶束,尽管其浓度     

Immersion behaviour of calcium polyphosphate in simulated body fluid

This work documents an investigation into the immersion behaviour of calcium polyphosphate (CPP) in simulated body fluid (SBF) for various periods. The results showed that with the increase of soaking time in SBF, a number of tiny particles were observed on the surface of samples by scanning electron microscope (SEM). The results of X-ray diffraction (XRD) indicated that the particles were contributed to apatite. And the changes of PO₄³⁻ and Ca²⁺ concentrations in SBF were detected by phospho-vanado-molybdate method and inductively coupled plasma atomic emission spectroscopy (ICP) methods respectively. The results indicated that the concentrations of PO₄³⁻ and Ca²⁺ in SBF reached the maximum value after 25 days of immersion, and then decreased with further increase of the soaking time. It is suggested that the degradation and ion exchange of CPP samples are dominant during the early stage of soaking, and then the precipitates begin to form and increase gradually as the soaking time increases. This study has demonstrated that apatite could be formed on the surface of CPP samples, and CPP would be used as bone substitution material.     

Cladding of titanium/fluorapatite composites onto Ti6Al4V substrate and the in vitro behaviour in the simulated body fluid

To improve the bioactivity of Ti6Al4V alloy, an innovative cladding method has been developed to bond a Ti/fluorapatite (FA) composite onto the alloy for load-bearing applications. With the aid of a silver interlayer and external pressure during sintering, a defect-free interface between the composite and the substrate was obtained. The fabricated materials were bioactive and could induce the nucleation and formation of bone-like carbonated apatite after immersed in the simulated body fluid (SBF). Functional ions, such as Ag⁺ and F⁻, were released from the materials during immersion, which could impart favourable activities for the implant. This work demonstrated that a simple and novel method could be applied to enhance functionalities of Ti alloys for load-bearing implant applications.     

太阳能玻璃表面高强度双层减反膜制备研究

用膜系设计软件设计了λ/4-λ/2的W型的双层减反射薄膜,优化了薄膜的光学常量,并使用溶胶-凝胶技术在玻璃基底上成功镀制了该双层折射率梯度的减反射薄膜.用椭圆偏振光谱仪、紫外-可见-近红外分光光度计、原子力显微镜等分析表征了薄膜的性能.结果表明,镀制了该双层薄膜的玻璃在400 nm～800 nm波段平均透过率增加了近6%,同时薄膜显示出了极佳的机械强度.     

Monodispersed Bioactive Glass Nanoparticles Enhance the Osteogenic Differentiation of Adipose‐Derived Stem Cells through Activating TGF‐Beta/Smad3 Signaling Pathway

It is important to understand the interaction mechanisms between nanomaterials and adipose‐derived stem cells for biomedical application. Nanoscale bioactive glass has positive effects on guiding osteoblasts differentiation and bone regeneration. However, the effects and molecular mechanism of monodispersed bioactive glass nanoparticles on the osteogenic differentiation of adipose‐derived stem cells are still not clear up to now. In this study, the effects and underlying molecular mechanism of monodispersed bioactive glass nanoparticles on the osteogenic differentiation of adipose‐derived stem cells are investigated in minute detail. The results show that nanoparticles (100–200 nm) can be absorbed by stem cells and is distributed in cytoplasm and nucleus. In both culture conditions (normal and osteoinductive), nanoparticles (80 µg mL⁻¹) can significantly enhance the osteogenic differentiation of stem cells through upregulating the alkaline phosphatase activity, osteogenic genes and protein expressions, as well as calcium deposition. Further study suggests that the activation of transforming growth factor‐beta/Smad3 signaling pathway plays an important role in the osteogenic differentiation of adipose‐derived stem cells enhanced by monodispersed nanoparticles. This study may have important implications for better understanding of stem cells fate induced by monodispersed nanoparticles and provide a promising approach toward stem cells‐based bone regeneration.     

Sb3+对Tb3+激活硅酸盐玻璃发光性能的影响

利用高温熔融法分别制备了Sb3 ,Tb3 单掺和共掺的硅酸盐发光玻璃,并分析了它们的光谱性质。根据对Sb3 和Tb3 掺杂硅酸盐玻璃的激发光谱、发射光谱和发光衰减时间等特性的分析,研究了澄清剂Sb2O3的加入对Tb3 激活硅酸盐玻璃发光性能的影响。结果表明,在紫外光激发下,Tb3 激活硅酸盐玻璃中存在Sb3 离子至Tb3 离子的能量传递,但能量传递效率较低,能量传递表现为Sb3 离子的3P1能级与Tb3 离子的5D3能级之间的能量无辐射共振转移。同时Sb3 离子的加入将在Sb3 离子和Tb3 离子的激发重叠区域(200～350nm)对Tb3 离子的激发产生不小的负面影响,尚不足以通过Sb3 离子至Tb3 离子的能量传递得以弥补。因此在使用Sb2O3作为Tb3 激活硅酸盐发光玻璃的澄清剂时,应当注意权衡Sb3 离子对Tb3 离子发光性能的影响。     

酞菁氯镓复合凝胶玻璃的谱学性能研究

采用溶胶-凝胶(Sol-Gel)湿化学工艺将酞菁氯镓(GaPcCl)掺入二氧化硅(SiO₂)凝胶玻璃基质,制备出均匀掺杂的GaPcCl复合凝胶玻璃,并对复合体系的红外光谱(IR)、紫外-可见吸收光谱(UV-Vis)及荧光光谱等谱学性能进行了测试。结果表明：GaPcCl的掺杂对凝胶玻璃基质的红外光谱没有产生显著影响;掺杂GaPcCl在复合体系中二聚体吸收峰的强度较其DMF溶液有所增大;掺杂GaPcCl在复合体系中荧光强度随浓度的增加远大于DMF溶液。     

Hologram Recording in Various Glass Plates by Corona Charging

We propose techniques of hologram replication in glass plates and reconstruction on another film by corona charging. A surface relief hologram on an azobenzene polymer film was recorded in the form of electric polarization in glass plates that include alkali cations by corona charging at high temperature. The hologram recorded in the glass plate is stable for more than 1 month at room temperature. After removal of the azobenzene polymer film from the plate, poly(methyl methacrylate) (PMMA) film was spin-coated onto the plate. The hologram recorded in the plate was reconstructed with the same surface relief structure on the PMMA film by corona charging again at 110°C.