浮法玻璃表面渗锡研究及电气石纳米薄膜制备与性能表征
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摘要
本篇论文工作分为两个方面。第一,针对浮法玻璃材料特定的渗锡缺陷,采用多种现代分析手段进行了渗锡形成机理的研究,对减轻渗锡的处理方法中的科学问题等进行了讨论,确认了新的定量渗锡测量的分析手段及表征方法,建立了判断出现浮法玻璃表面钢化虹彩的渗锡量阈值;第二,针对目前电磁屏蔽玻璃透光性与高频段屏蔽效能无法兼顾的问题,结合纳米电气石材料具有的自发极化特征,设计了宽频带电磁屏蔽玻璃的功能材料结构,并对靶材及成膜机制开展了系列实验研究,确认了电气石被沉积在镀有导电膜的玻璃表面,对薄膜性能进行了初步测试。
研究结果表明,可以用XRF(X-Ray Fluorescence spectroscopy)强度测量值表征浮法玻璃表面渗锡含量。用XPS(X-ray Photoelectron Spectroscopy)方法明确了浮法玻璃下表面中的锡元素以Sn0、Sn2+、Sn4+状态存在,确定了各价态的锡元素在渗入玻璃中的比例。渗锡量中Sn2+的含量决定着是否产生钢化虹彩以及其程度,XRF锡计数可以用来近似表征Sn2+的含量,也确定产生虹彩现象存在渗锡量的临界值。通过光致发光(Photoluminescence, PL)分析方法,找出了浮法玻璃表面渗锡的荧光激发发射特征谱,并建立了与XRF的定量关系。在第一性原理的基础上,分别按CaSi4O8体系、MgSi4O8体系计算了Mg、Fe和Sn离子替换Ca离子前后体系结构能量的变化。以化学配位理论为出发点,讨论了在玻璃成形的高温环境中,可能的离子替换是所产生的系统结构能量与初始结构能量差较小的容易发生,而那些替换完成后系统结构能量变得较高的状态相对较难发生,在结构能量接近的情况下存在多种替换反应同时发生的可能性。对计算结果的分析表明,当玻璃体中含铁量较高,或者金属锡液中加入微量铁的情况下,可以阻止锡元素向玻璃内部的扩散。经对SO2处理前后浮法玻璃下表面样品的XRF和EDX(Energy Dispersive X-ray spectroscopy)分析表明,未能找到浮法玻璃下表面内锡离子在SO2气氛的作用下的产物和锡离子进一步扩散的特征。采用多种分析方法对过渡辊材料的样品表面进行的分析,表明热辊表面硫含量按着非线性指数规律增加,热辊样品表面形成了具有层状结构的疏松的FeS层,可以起到润滑作用。但SO2熏蒸热辊时间和加大浓度,对热辊表面润滑作用不会进一步增加,对浮法玻璃生产环境有一定污染。SO2气体与浮法玻璃表面富集的碱金属氧化物反应形成硫酸盐,起到了抗发霉作用。
系统研究了镀有ITO导电膜的透明玻璃的电磁屏蔽特征,ITO玻璃薄膜对电磁波的反射率在低频段(<1 GHe)保持在97%以上,但在高频波段,ITO镀膜玻璃的屏蔽效能明显下降,典型值为在600 MHz,下降到43 dB,在4 GHz,下降到35.5 dB。在明确电气石热学性能的情况下,利用离子束溅射沉积方法,选择合适的条件,在在线Low-E玻璃表面实现电气石的纳米化镀层,并表现出特有的自发极化特征。
This paper is mainly composed of two parts. Firstly, focusing on the mechanisms of the formed tin-related defects in float glass and the methods to alleviate them, new analyzing and assigning methods were developed to carry out quantitative measurement accurately. A new critical value of tin content was also proposed and affirmed as the threshold of the appearance of bloom phenomenon during further quenching process on float glass. Secondly, due to the problems of traditional electromagnetic shielding glass in achieving high visible light transparency and high shielding effectness in high frequency region simultaneously, a new functional material structure based on the self-polarization of nanometer-scaled tourmaline was proposed to abtain better shielding effectness in a more wider electromagnetic wave range, where system studies were dedicated to the target and deposition mechanisms of thin films to affirm the deposition of nanometer-sized tourmaline film on glass substrate. After that primary investigations were conducted to analysze the properties of the as-prepared thin films.
The results displayed that the XRF (X-Ray Fluorescence spectroscopy) can be used to investigate the tin content in float glass, while XPS (X-ray Photoelectron Spectroscopy) was used to affirm the existing stated and their relative proportions of Sn0, Sn2+ and Sn4+. The content of Sn2+ will decide the appearance and the degree of bloom phenomenon. Therefore, XRF intensity of tin can be used approximatively as the staff of Sn2+ content and the further threshold of the appearance of bloom phenomenon during quenching process on float glass. PL (photoluminescence) analysis was used to investigate to characterictic PL excitation and emission spectra of tin in float glass. The quantitative relationship between PL intensity and XRF intensity of tin in float glass was also affirmed. Based on first principles calculations, the varieties of total energies of the models incorporated as CaSi4O8 system and MgSi4O8 system with Ca displaced by Mg, Fe or Sn or other elements were calculated. With chemical ligand field theory, the possible ion exchange reactions happened at high tempereture were estimated by evaluating the energy gap between the models before and after element relpacing. Tt is believed that the replace will not happen if the energy gap is huge, on the other hand, several replaces may exist simultaneously when the energies are very near and small. The results exhibited that it would block the duffusion of tin into float glass by high Fe content in float glass or the minor accession of Fe in tin liquid. XRF and EDX (Energy Dispersive X-ray spectroscopy) analysis on float glass samples maintained in SO2 atmosphere with different treating times revealed no proof for further diffusion of tin in the tin-bath surface of float glass. The analysis by several methods showed that the S content in the surface of transitional roll increased exponentially, where layered loose FeS formed and acted as lubricant. However, prolonging the treating time or elevating the SO2 concentration won’t enhance the lubricating effect of the FeS layer, but only causing the pollution for the environment. The sulphate formed by the reaction between SO2 and the alkali oxide enriched near the surface of float glass will help the glass from going moldy.
The electromagnetic shielding behavior of transparent glass covered with ITO conducting film was investigated systematically. The reflectness of this kind of ITO glass in low frequency region (<1 GHe ) maintains above 97%, but at high frequency region the shielding effectness drops remarkablly. The typical value of the shielding effectness at 600 MHz and 4 GHz were 43 dB and 35.5 dB, respectively. On the basic of comprehension of the calorifics properties of tourmaline, proper measurements were taken to obtain nanometer-sized tourmaline film successfully fabricated by ion-beam sputtering deposition on on-line Low-E glass substrate and gain the characteristic self-polarization of the as-prepared film.
研究结果表明,可以用XRF(X-Ray Fluorescence spectroscopy)强度测量值表征浮法玻璃表面渗锡含量。用XPS(X-ray Photoelectron Spectroscopy)方法明确了浮法玻璃下表面中的锡元素以Sn0、Sn2+、Sn4+状态存在,确定了各价态的锡元素在渗入玻璃中的比例。渗锡量中Sn2+的含量决定着是否产生钢化虹彩以及其程度,XRF锡计数可以用来近似表征Sn2+的含量,也确定产生虹彩现象存在渗锡量的临界值。通过光致发光(Photoluminescence, PL)分析方法,找出了浮法玻璃表面渗锡的荧光激发发射特征谱,并建立了与XRF的定量关系。在第一性原理的基础上,分别按CaSi4O8体系、MgSi4O8体系计算了Mg、Fe和Sn离子替换Ca离子前后体系结构能量的变化。以化学配位理论为出发点,讨论了在玻璃成形的高温环境中,可能的离子替换是所产生的系统结构能量与初始结构能量差较小的容易发生,而那些替换完成后系统结构能量变得较高的状态相对较难发生,在结构能量接近的情况下存在多种替换反应同时发生的可能性。对计算结果的分析表明,当玻璃体中含铁量较高,或者金属锡液中加入微量铁的情况下,可以阻止锡元素向玻璃内部的扩散。经对SO2处理前后浮法玻璃下表面样品的XRF和EDX(Energy Dispersive X-ray spectroscopy)分析表明,未能找到浮法玻璃下表面内锡离子在SO2气氛的作用下的产物和锡离子进一步扩散的特征。采用多种分析方法对过渡辊材料的样品表面进行的分析,表明热辊表面硫含量按着非线性指数规律增加,热辊样品表面形成了具有层状结构的疏松的FeS层,可以起到润滑作用。但SO2熏蒸热辊时间和加大浓度,对热辊表面润滑作用不会进一步增加,对浮法玻璃生产环境有一定污染。SO2气体与浮法玻璃表面富集的碱金属氧化物反应形成硫酸盐,起到了抗发霉作用。
系统研究了镀有ITO导电膜的透明玻璃的电磁屏蔽特征,ITO玻璃薄膜对电磁波的反射率在低频段(<1 GHe)保持在97%以上,但在高频波段,ITO镀膜玻璃的屏蔽效能明显下降,典型值为在600 MHz,下降到43 dB,在4 GHz,下降到35.5 dB。在明确电气石热学性能的情况下,利用离子束溅射沉积方法,选择合适的条件,在在线Low-E玻璃表面实现电气石的纳米化镀层,并表现出特有的自发极化特征。
This paper is mainly composed of two parts. Firstly, focusing on the mechanisms of the formed tin-related defects in float glass and the methods to alleviate them, new analyzing and assigning methods were developed to carry out quantitative measurement accurately. A new critical value of tin content was also proposed and affirmed as the threshold of the appearance of bloom phenomenon during further quenching process on float glass. Secondly, due to the problems of traditional electromagnetic shielding glass in achieving high visible light transparency and high shielding effectness in high frequency region simultaneously, a new functional material structure based on the self-polarization of nanometer-scaled tourmaline was proposed to abtain better shielding effectness in a more wider electromagnetic wave range, where system studies were dedicated to the target and deposition mechanisms of thin films to affirm the deposition of nanometer-sized tourmaline film on glass substrate. After that primary investigations were conducted to analysze the properties of the as-prepared thin films.
The results displayed that the XRF (X-Ray Fluorescence spectroscopy) can be used to investigate the tin content in float glass, while XPS (X-ray Photoelectron Spectroscopy) was used to affirm the existing stated and their relative proportions of Sn0, Sn2+ and Sn4+. The content of Sn2+ will decide the appearance and the degree of bloom phenomenon. Therefore, XRF intensity of tin can be used approximatively as the staff of Sn2+ content and the further threshold of the appearance of bloom phenomenon during quenching process on float glass. PL (photoluminescence) analysis was used to investigate to characterictic PL excitation and emission spectra of tin in float glass. The quantitative relationship between PL intensity and XRF intensity of tin in float glass was also affirmed. Based on first principles calculations, the varieties of total energies of the models incorporated as CaSi4O8 system and MgSi4O8 system with Ca displaced by Mg, Fe or Sn or other elements were calculated. With chemical ligand field theory, the possible ion exchange reactions happened at high tempereture were estimated by evaluating the energy gap between the models before and after element relpacing. Tt is believed that the replace will not happen if the energy gap is huge, on the other hand, several replaces may exist simultaneously when the energies are very near and small. The results exhibited that it would block the duffusion of tin into float glass by high Fe content in float glass or the minor accession of Fe in tin liquid. XRF and EDX (Energy Dispersive X-ray spectroscopy) analysis on float glass samples maintained in SO2 atmosphere with different treating times revealed no proof for further diffusion of tin in the tin-bath surface of float glass. The analysis by several methods showed that the S content in the surface of transitional roll increased exponentially, where layered loose FeS formed and acted as lubricant. However, prolonging the treating time or elevating the SO2 concentration won’t enhance the lubricating effect of the FeS layer, but only causing the pollution for the environment. The sulphate formed by the reaction between SO2 and the alkali oxide enriched near the surface of float glass will help the glass from going moldy.
The electromagnetic shielding behavior of transparent glass covered with ITO conducting film was investigated systematically. The reflectness of this kind of ITO glass in low frequency region (<1 GHe ) maintains above 97%, but at high frequency region the shielding effectness drops remarkablly. The typical value of the shielding effectness at 600 MHz and 4 GHz were 43 dB and 35.5 dB, respectively. On the basic of comprehension of the calorifics properties of tourmaline, proper measurements were taken to obtain nanometer-sized tourmaline film successfully fabricated by ion-beam sputtering deposition on on-line Low-E glass substrate and gain the characteristic self-polarization of the as-prepared film.
引文
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