以二氧化硅为基体的新型传感材料的制备、表征和应用研究
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摘要
对于被掺杂、吸附或镶嵌的传感物质而言二氧化硅是一个优良的基体材料,它具有较高的热稳定性和化学稳定性、高绝缘性、对可见光透明等优点,目前已成为重要的催化剂载体和高化学活性的纳米材料的承载基体,在研究和生产中有广泛的应用。
硅胶作为一种重要的二氧化硅材料具有多孔性和高吸附性的特点。具有高吸附能力的多孔硅胶已被直接运用于湿度传感器,同时也被广泛应用于各种溶剂中微量成分的富集检测。而更广泛的运用于传感器的是掺杂有或固载有各种传感物质的硅胶材料。本文研究了具有色度传感特性和磷光传感特性的含钒硅胶干凝胶。目前掺杂或未掺杂的含钒硅胶的干凝胶、薄膜和块体材料的研究已经引起了极大的关注和兴趣,因为这种材料在催化、热致变色、电致变色和信号转换设备等各个领域有着广阔的用途。在上世纪90年代,含钒硅胶干凝胶遇水变红的特性已经被用于湿度传感器的研制,而这种材料在水存在的条件下被乙醇还原而变成黄绿色的特性第一次在本研究中用于乙醇中微量水分的色度传感研究。本文研究的含钒硅胶干凝胶以104.5 mL正硅酸乙酯、1.4259 g偏钒酸铵、117 mL乙醇和108 mL二次去离子水为原料经过溶胶凝胶的方法制成,具有廉价低毒的优点。在制备过程中未引入酸、碱等加快凝胶速度的催化剂,使样品具有很高的纯度,这一优点简化了制备工艺和对样品的颜色起源以及磷光起源的分析。实验发现经过在500℃下焙烧l小时处理后的含钒硅胶干凝胶薄片呈现无色透明状,当冷却后的干凝胶薄片接触环境空气时,薄片在3秒钟内变为橙红色,显示了本实验制备的含钒硅胶材料具有很高的空气湿度传感灵敏度和传感速率。热失重分析显示薄片能吸收约为自身重量21%的水份,并且在100℃下加热,能够除去所有物理吸附的水份,表明这种湿度指示材料很容易再生。光学显微照片显示薄片表面有大量孔洞,表明薄片具有高吸附能力。电子自旋共振实验发现含钒硅胶干凝胶薄片中的V5+在水存在的条件下被乙醇还原成特征颜色为蓝绿色的四价含氧钒离子[VO(H2O)5]2+。浸泡在含水乙醇中的薄片同时生成红色的络合了两个水分子的五价钒离子中心生色团和蓝绿色的[VO(H2O)5]2+生色团。红色和蓝绿色混合成黄绿色,黄绿色的互补色是蓝色。本研究运用基于MATLAB的自编程序提取了浸泡在不同水含量的乙醇溶液中的含钒硅胶干凝胶薄片的照片图像的B原色强度数值,绘制了B值与乙醇溶液中水分含量的关系曲线,发现B值随着水含量单调变化。通过测定含钒硅胶干凝胶薄片的照片图像的B值可以定量检测乙醇溶液中的水分含量,水浓度的检测下限小于1%。作为一种色度测量方法,本研究使用的设备是普通数码相机,省去了紫外一可见分光光谱仪或红外吸收光谱仪等专业色度分析仪器的昂贵费用,同时有具有好的分析效果。
实验发现经过在800℃和1100℃下焙烧1小时的含钒硅胶干凝胶薄片能够发射峰值为527nm(800℃)和537nm(1100℃)的强烈磷光。光学显微照片显示经过800℃焙烧的薄片表面有大量孔洞,而在1100℃下焙烧过的薄片表面致密,呈现玻璃态。水、乙醚,硫代硫酸钠和氢氟酸能够渗入经过800℃焙烧的薄片内部猝灭其磷光。这个现象表明经过在800℃下焙烧的含钒硅胶干凝胶薄片可以用作水、乙醚,硫代硫酸钠和氢氟酸的磷光传感材料。实验发现,经过500℃焙烧的薄片没有磷光,而在1100℃下焙烧的薄片的磷光比在800℃下焙烧的更强烈。这个实验现象不能用已有的理论解释。结合在TEM实验中发现了五氧化二钒纳米晶的实验事实,本文对含钒硅胶干凝胶薄片的磷光发射机理和水对磷光猝灭机理的解释做了新的尝试:含钒硅胶干凝胶薄片的磷光发射来自于具有量子尺寸效应的五氧化二钒纳米晶;水对磷光的猝灭作用来自于渗透了水的Si02基体对五氧化二钒纳米晶的介电限域效应。
自上世纪八十年代末纳米科技兴起以来,人们对嵌入二氧化硅基体中的纳米材料的奇异的物理、化学性质展开了深入的研究。嵌入二氧化硅基体中的锗纳米晶展现了有巨大应用前景的新颖的光电性质,有望成为未来纳米电子学和纳米光学的一个重要基础材料,从而引起了研究者的普遍重视。迄今,在以往有关嵌入SiO2膜中Ge纳米晶(nc-Ge)制备方法(如离子注入法、磁控射频溅射法、化学气相沉积法,溶胶凝胶法等)的报道中,一般需附加400℃以上温度的退火处理才可形成Ge纳米晶,这会增加Ge纳米晶制备的技术复杂性和成本。而且对离子注入方法来说,以往研究中使用的离子注入剂量不高,低于l×1017cm2,使得纳米晶浓度过低,光荧光强度不高。目前高剂量注入极端条件下产生的新现象和新物性还不清楚,有待开展研究。本研究首次报道了不经过退火处理,通过大幅提高Ge离子注入量直接制备nc-Ge的方法,对Ge纳米晶的形成机理进行了实验研究和讨论,对镶嵌nc-Ge的Si02膜的光致发光谱进行了实验研究,并对其发光机理进行了探讨。本研究提出的纳米晶制备技术可精确控制锗纳米晶的分布和尺寸,可用于高质量锗纳米晶的制备。实验中观察到的锗纳米晶的发光特性可用于射线剂量的光学探测。
Silicon dioxide is a kind of excellent substrate material for the adulterated or adsorbed or embedded sensitive species, which has some advantages as the substate, such as inert to reactant, heat stability, high insulative ability and great transparency, and has been widely applied to research and industry as the important substrate of catalyst and the vivacious material at nanometer scale.
Silica gel is an important kind of silicon oxide with porous structure and high adsorptive ability. Pure porous silica gel has been directly applied to humidity measurement and the detection of trace substance in solvent, after which had been adsorbed and condensed by silica gel. However, most of silica gels used in sensors have to load special sensitive species to detect the analytes. This thesis studied the fabrication of vanadia-silica xerogel and its application for chroma sensor and phosphorescence sensor. Synthesis and stabilization of pure and doped vanadia-silica xerogels, either in the shape of thin films or bulk materials, have attracted considerable attention due to their diverse applications in thermochromic, electrochromic and switching devices. In 1990's, researchers had developed humidity sensor with vanadia-silica xerogels as the sensitive element which could become red when adsorbing water vapour in air. In this study, it is first reported the fabrication of the sensor based on the color change of vanadia-silica xerogels slice due to the reduction of V5+ ions in the xerogel slice by ethanol with water's participation, which was used to detect the trace water in ethanol. The vanadia-siiica xerogels slice is low-cost, low toxic, mass produce, easy to fabricate and less chemicals consumption, prepared simply with 104.5 mL tetraethyl orthosilicate, 1.4259 g ammonium metavanadate, 117 mL ethanol and 108 mL redistilled water. During the gelation of colloid, no acidic or alkaline catalyst was employed, which ensures the purity of vanadia-silica xerogels and simplifys the analysis of chromophore and phosphorescence resource. It can be observed that the vanadia-silica xerogels slice heated at 500°C for 1 h is colorless and transparent. When the cooled slice expose to ambient air, it turn red within 3 seconds. This behavior suggests that the slice has ultra sensitivity and excellent response speed toward humidity. With thermogravimetric analysis experiment, it's discovered that the maximal weight of water adsorbed by the slice was about 21% (w/w) of that of slice and that the slice would be completely dehydrated when heated at 100°C, which indicates the humidity sensing ability of the slice is reproducible. The microscopic photograph of the slice reveals that the adsorption ability of the slice comes from its porous structure. The results of ESR measurement shows V5+ in the slice could be deoxidized to [VO(H2O)5]2+ which is green blue by ethanol on condition that water participated in the reaction. When the xerogel slices are soaked in ethanol solution containing water, the green blue [VO(H2O)5]2+ and the red pseudooctahedral oxovanadium(V) centers produced by the coordination of two water molecules to the vanadium metal center will be formed, and then the color of the slice will turn into green yellow whose complementary color is blue. In this reseach work, B values of the images captured by a commecial digital camera of the slices soaked in ethanol solution with diverse water content were collected by home made program based on MATLAB software, and then the relationship curve of B value and water content was achieved. It's found that the B value monotonously increased with water content decreasing. This relationship can be applied to the detection of trace water in ethanol solution with detection limit of 1 v/v %. The detection method of water content used in this work only need a family digital camera instead of expensive UV-Vis or IR. spectrophotometer, simultaneously owning a good measurement precision.
Furthermore, it's found that the vanadia-silica xerogel slice could emit phosphorescence with the wavelength peaked at 527 nm and 537 nm after heated at 800°C and 1100°C for 1 hour respectively. Microscopic photograph shows the porous structure of the surface of the slice after heated at 800°C, while the surface of the slice is glassy after heated at 1100°C. Water, ether, sodium hyposulphite aqueous solution and hydrofluoric acid can penetrate into the slice heated at 800°C and quench its phosphorescence, suggesting that the slice heated at 800°C can be used as phosphorescence sensor for water, ether, sodium hyposulphite aqueous solution or hydrofluoric acid. The experiments demonstrated that the slice couldn't emit phosphorescence heated at 500°C, and that the phosphorescence intensity of the slice heated at 1100°C was larger than that of 800°C sample. A possible interpretation is presented based on the observation of V2O5 nanocrystal in the slice heated at 1100°C in TEM experiment. The quantum size effect of V2O5 nanocrystal leads to its phosphorescence emission, and the dielectric confinement effect of the SiO2 matrix surrounding V2O5 nanocrystal leads to the phosphorescence quenching.
Since the end of 1980’s, the novel physical and chemical properties of nanometer materials embedded in SiO2 matrix have been intensively studied. Ge nanocrystal embedded in SiO2 matrix has shown its potential applications due to its novel optical and electrical properties, and will be an important basic material of nanoelectronics and nanooptics components. So far, in the reported preparation methods of nano-crystalline Ge (nc-Ge) embedded in SiO2 matrix mainly inclouding magnetron co-sputtering, chemical vapor deposition (CVD), ion implantation and sol-gel method, heat process at temperature above 400°C is a necessary procedure for preducing nanocrystal, which will increase the preparation cost and difficulty. As to ion implantation method, because the ion fluence of 1×1017cm-2 has greatly exceeded a solid surface atomic density (～1×1015 cm-2),so the ion implantation with the fluence above 1×1017 cm-2 was less carried out for nano-crystalline Ge preparation. As a result, the density of nano-particles is low and the intensity of corresponding photoluminescence is weak. It has not been clarified whether Ge nanocrystal with high-intensity photoluminescence can be prepared by ion implantation with higher fluence than 1×1017 cm-2. In this thesis, a new preparation method is reported, by which, nc-Ge can be directly produced by high dose ion implantation without subsequent annealing. The mechanisms of the formation and the fluorescence emission of nc-Ge are discussed. The preparation technique of nc-Ge used in this reseach work can be applied to produce high quality nc-Ge, owning to the advantages of the precise control of the depth distribution and the required density of nc-Ge in matrix by changing ion energy and fluence. The photoluminescence property of nc-Ge can be applied to fluorescence sensor for radiation fluence detection.
硅胶作为一种重要的二氧化硅材料具有多孔性和高吸附性的特点。具有高吸附能力的多孔硅胶已被直接运用于湿度传感器,同时也被广泛应用于各种溶剂中微量成分的富集检测。而更广泛的运用于传感器的是掺杂有或固载有各种传感物质的硅胶材料。本文研究了具有色度传感特性和磷光传感特性的含钒硅胶干凝胶。目前掺杂或未掺杂的含钒硅胶的干凝胶、薄膜和块体材料的研究已经引起了极大的关注和兴趣,因为这种材料在催化、热致变色、电致变色和信号转换设备等各个领域有着广阔的用途。在上世纪90年代,含钒硅胶干凝胶遇水变红的特性已经被用于湿度传感器的研制,而这种材料在水存在的条件下被乙醇还原而变成黄绿色的特性第一次在本研究中用于乙醇中微量水分的色度传感研究。本文研究的含钒硅胶干凝胶以104.5 mL正硅酸乙酯、1.4259 g偏钒酸铵、117 mL乙醇和108 mL二次去离子水为原料经过溶胶凝胶的方法制成,具有廉价低毒的优点。在制备过程中未引入酸、碱等加快凝胶速度的催化剂,使样品具有很高的纯度,这一优点简化了制备工艺和对样品的颜色起源以及磷光起源的分析。实验发现经过在500℃下焙烧l小时处理后的含钒硅胶干凝胶薄片呈现无色透明状,当冷却后的干凝胶薄片接触环境空气时,薄片在3秒钟内变为橙红色,显示了本实验制备的含钒硅胶材料具有很高的空气湿度传感灵敏度和传感速率。热失重分析显示薄片能吸收约为自身重量21%的水份,并且在100℃下加热,能够除去所有物理吸附的水份,表明这种湿度指示材料很容易再生。光学显微照片显示薄片表面有大量孔洞,表明薄片具有高吸附能力。电子自旋共振实验发现含钒硅胶干凝胶薄片中的V5+在水存在的条件下被乙醇还原成特征颜色为蓝绿色的四价含氧钒离子[VO(H2O)5]2+。浸泡在含水乙醇中的薄片同时生成红色的络合了两个水分子的五价钒离子中心生色团和蓝绿色的[VO(H2O)5]2+生色团。红色和蓝绿色混合成黄绿色,黄绿色的互补色是蓝色。本研究运用基于MATLAB的自编程序提取了浸泡在不同水含量的乙醇溶液中的含钒硅胶干凝胶薄片的照片图像的B原色强度数值,绘制了B值与乙醇溶液中水分含量的关系曲线,发现B值随着水含量单调变化。通过测定含钒硅胶干凝胶薄片的照片图像的B值可以定量检测乙醇溶液中的水分含量,水浓度的检测下限小于1%。作为一种色度测量方法,本研究使用的设备是普通数码相机,省去了紫外一可见分光光谱仪或红外吸收光谱仪等专业色度分析仪器的昂贵费用,同时有具有好的分析效果。
实验发现经过在800℃和1100℃下焙烧1小时的含钒硅胶干凝胶薄片能够发射峰值为527nm(800℃)和537nm(1100℃)的强烈磷光。光学显微照片显示经过800℃焙烧的薄片表面有大量孔洞,而在1100℃下焙烧过的薄片表面致密,呈现玻璃态。水、乙醚,硫代硫酸钠和氢氟酸能够渗入经过800℃焙烧的薄片内部猝灭其磷光。这个现象表明经过在800℃下焙烧的含钒硅胶干凝胶薄片可以用作水、乙醚,硫代硫酸钠和氢氟酸的磷光传感材料。实验发现,经过500℃焙烧的薄片没有磷光,而在1100℃下焙烧的薄片的磷光比在800℃下焙烧的更强烈。这个实验现象不能用已有的理论解释。结合在TEM实验中发现了五氧化二钒纳米晶的实验事实,本文对含钒硅胶干凝胶薄片的磷光发射机理和水对磷光猝灭机理的解释做了新的尝试:含钒硅胶干凝胶薄片的磷光发射来自于具有量子尺寸效应的五氧化二钒纳米晶;水对磷光的猝灭作用来自于渗透了水的Si02基体对五氧化二钒纳米晶的介电限域效应。
自上世纪八十年代末纳米科技兴起以来,人们对嵌入二氧化硅基体中的纳米材料的奇异的物理、化学性质展开了深入的研究。嵌入二氧化硅基体中的锗纳米晶展现了有巨大应用前景的新颖的光电性质,有望成为未来纳米电子学和纳米光学的一个重要基础材料,从而引起了研究者的普遍重视。迄今,在以往有关嵌入SiO2膜中Ge纳米晶(nc-Ge)制备方法(如离子注入法、磁控射频溅射法、化学气相沉积法,溶胶凝胶法等)的报道中,一般需附加400℃以上温度的退火处理才可形成Ge纳米晶,这会增加Ge纳米晶制备的技术复杂性和成本。而且对离子注入方法来说,以往研究中使用的离子注入剂量不高,低于l×1017cm2,使得纳米晶浓度过低,光荧光强度不高。目前高剂量注入极端条件下产生的新现象和新物性还不清楚,有待开展研究。本研究首次报道了不经过退火处理,通过大幅提高Ge离子注入量直接制备nc-Ge的方法,对Ge纳米晶的形成机理进行了实验研究和讨论,对镶嵌nc-Ge的Si02膜的光致发光谱进行了实验研究,并对其发光机理进行了探讨。本研究提出的纳米晶制备技术可精确控制锗纳米晶的分布和尺寸,可用于高质量锗纳米晶的制备。实验中观察到的锗纳米晶的发光特性可用于射线剂量的光学探测。
Silicon dioxide is a kind of excellent substrate material for the adulterated or adsorbed or embedded sensitive species, which has some advantages as the substate, such as inert to reactant, heat stability, high insulative ability and great transparency, and has been widely applied to research and industry as the important substrate of catalyst and the vivacious material at nanometer scale.
Silica gel is an important kind of silicon oxide with porous structure and high adsorptive ability. Pure porous silica gel has been directly applied to humidity measurement and the detection of trace substance in solvent, after which had been adsorbed and condensed by silica gel. However, most of silica gels used in sensors have to load special sensitive species to detect the analytes. This thesis studied the fabrication of vanadia-silica xerogel and its application for chroma sensor and phosphorescence sensor. Synthesis and stabilization of pure and doped vanadia-silica xerogels, either in the shape of thin films or bulk materials, have attracted considerable attention due to their diverse applications in thermochromic, electrochromic and switching devices. In 1990's, researchers had developed humidity sensor with vanadia-silica xerogels as the sensitive element which could become red when adsorbing water vapour in air. In this study, it is first reported the fabrication of the sensor based on the color change of vanadia-silica xerogels slice due to the reduction of V5+ ions in the xerogel slice by ethanol with water's participation, which was used to detect the trace water in ethanol. The vanadia-siiica xerogels slice is low-cost, low toxic, mass produce, easy to fabricate and less chemicals consumption, prepared simply with 104.5 mL tetraethyl orthosilicate, 1.4259 g ammonium metavanadate, 117 mL ethanol and 108 mL redistilled water. During the gelation of colloid, no acidic or alkaline catalyst was employed, which ensures the purity of vanadia-silica xerogels and simplifys the analysis of chromophore and phosphorescence resource. It can be observed that the vanadia-silica xerogels slice heated at 500°C for 1 h is colorless and transparent. When the cooled slice expose to ambient air, it turn red within 3 seconds. This behavior suggests that the slice has ultra sensitivity and excellent response speed toward humidity. With thermogravimetric analysis experiment, it's discovered that the maximal weight of water adsorbed by the slice was about 21% (w/w) of that of slice and that the slice would be completely dehydrated when heated at 100°C, which indicates the humidity sensing ability of the slice is reproducible. The microscopic photograph of the slice reveals that the adsorption ability of the slice comes from its porous structure. The results of ESR measurement shows V5+ in the slice could be deoxidized to [VO(H2O)5]2+ which is green blue by ethanol on condition that water participated in the reaction. When the xerogel slices are soaked in ethanol solution containing water, the green blue [VO(H2O)5]2+ and the red pseudooctahedral oxovanadium(V) centers produced by the coordination of two water molecules to the vanadium metal center will be formed, and then the color of the slice will turn into green yellow whose complementary color is blue. In this reseach work, B values of the images captured by a commecial digital camera of the slices soaked in ethanol solution with diverse water content were collected by home made program based on MATLAB software, and then the relationship curve of B value and water content was achieved. It's found that the B value monotonously increased with water content decreasing. This relationship can be applied to the detection of trace water in ethanol solution with detection limit of 1 v/v %. The detection method of water content used in this work only need a family digital camera instead of expensive UV-Vis or IR. spectrophotometer, simultaneously owning a good measurement precision.
Furthermore, it's found that the vanadia-silica xerogel slice could emit phosphorescence with the wavelength peaked at 527 nm and 537 nm after heated at 800°C and 1100°C for 1 hour respectively. Microscopic photograph shows the porous structure of the surface of the slice after heated at 800°C, while the surface of the slice is glassy after heated at 1100°C. Water, ether, sodium hyposulphite aqueous solution and hydrofluoric acid can penetrate into the slice heated at 800°C and quench its phosphorescence, suggesting that the slice heated at 800°C can be used as phosphorescence sensor for water, ether, sodium hyposulphite aqueous solution or hydrofluoric acid. The experiments demonstrated that the slice couldn't emit phosphorescence heated at 500°C, and that the phosphorescence intensity of the slice heated at 1100°C was larger than that of 800°C sample. A possible interpretation is presented based on the observation of V2O5 nanocrystal in the slice heated at 1100°C in TEM experiment. The quantum size effect of V2O5 nanocrystal leads to its phosphorescence emission, and the dielectric confinement effect of the SiO2 matrix surrounding V2O5 nanocrystal leads to the phosphorescence quenching.
Since the end of 1980’s, the novel physical and chemical properties of nanometer materials embedded in SiO2 matrix have been intensively studied. Ge nanocrystal embedded in SiO2 matrix has shown its potential applications due to its novel optical and electrical properties, and will be an important basic material of nanoelectronics and nanooptics components. So far, in the reported preparation methods of nano-crystalline Ge (nc-Ge) embedded in SiO2 matrix mainly inclouding magnetron co-sputtering, chemical vapor deposition (CVD), ion implantation and sol-gel method, heat process at temperature above 400°C is a necessary procedure for preducing nanocrystal, which will increase the preparation cost and difficulty. As to ion implantation method, because the ion fluence of 1×1017cm-2 has greatly exceeded a solid surface atomic density (～1×1015 cm-2),so the ion implantation with the fluence above 1×1017 cm-2 was less carried out for nano-crystalline Ge preparation. As a result, the density of nano-particles is low and the intensity of corresponding photoluminescence is weak. It has not been clarified whether Ge nanocrystal with high-intensity photoluminescence can be prepared by ion implantation with higher fluence than 1×1017 cm-2. In this thesis, a new preparation method is reported, by which, nc-Ge can be directly produced by high dose ion implantation without subsequent annealing. The mechanisms of the formation and the fluorescence emission of nc-Ge are discussed. The preparation technique of nc-Ge used in this reseach work can be applied to produce high quality nc-Ge, owning to the advantages of the precise control of the depth distribution and the required density of nc-Ge in matrix by changing ion energy and fluence. The photoluminescence property of nc-Ge can be applied to fluorescence sensor for radiation fluence detection.
引文
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