摘要
低辐射薄膜的热稳定性能具有重要的理论意义和实用价值，但尚未得到系统地研究和表征。本文以化学气相沉积法制备的掺杂F的SnO_2（FTO）低辐射薄膜和磁控溅射法制备的Ag基低辐射薄膜为研究对象，分别在马弗炉和钢化炉中进行后期高温处理，采用X射线衍射仪、场发射扫描电镜、原子力显微镜、紫外-可见分光光度计和综合物理性能测试系统研究了其结构、形貌、光电性质的温度和时间效应。采用显微拉曼光谱仪研究了FTO薄膜的室温光致发光机理。通过X光电子能谱分析了薄膜中元素的分布情况，探讨了薄膜电学性能的恶化机理。主要研究结果如下：
具有SnO_2:F/SiO_xCy膜系结构的FTO低辐射薄膜具有良好的高温热稳定性，最高耐热温度为600℃，最长耐热时间为15min，当超过此条件时，光电性能恶化。FTO薄膜内部的主要组成为非化学计量比的SnO_(2-x):F（x≈0.8~0.9），是金红石结构的多晶SnO_2，以（200）晶面为最明显的择优取向。在325~650nm之间，FTO薄膜的室温PL谱明显地分为三个区域，紫外发光峰是激发态下电子空穴对的复合发光。385.20nm处的发光峰与取代位置的氟相关，409.33nm和441.69nm处的发光峰分别与带一个正电荷的氧空位VO和带两个正电荷的氧空位VO相关。蓝绿色发光峰与表面态、结构缺陷等相关。薄膜内部[O]/[Sn]比受高温钢化的影响较小，对导电性恶化的贡献较小。随钢化温度的升高和时间的延长，薄膜表层缺乏状态氧的相对含量逐渐降低，FTO和SiO_xCy阻挡层之间的界面扩散层中Si-O键相对含量逐渐增加，这一变化趋势与电阻率的升高一致。
与玻璃/TiO_2/ZnO/Ag/NiCrO_x/SnO_2/Si_3N_4膜层结构的Ag基薄膜相比，在功能层Ag层下面预先沉积1.1nm NiCrO_x和12nm Si_3N_4得到的具有玻璃/Si_3N_4/TiO_2/NiCrO_x/ZnO/Ag/NiCrO_x/SnO_2/Si_3N_4膜层结构的改良型Ag基薄膜的热稳定性可提高至600℃，在温度为60±1℃，相对湿度为90±2%条件下进行水雾处理后，改良型Ag基薄膜的耐水性可提高至17天。Ag基薄膜是由结晶的Ag层以及无定形的其他膜层组成，当热处理温度高于600℃时，Ag层的择优取向由（111）晶面向（220）晶面转换。改良型Ag基薄膜在675±25℃钢化炉中钢化6min后，Ag中出现少量的Ag2O。在Ag层以下的NiCrO_x膜层中，与氧成键的CrI与无定形CrII的相对含量由钢化前的0.62增大到钢化后的0.74，说明Ag层的氧化是底层氧的扩散所致。钢化6min后，功能层Ag层致密度和结晶度的提高对于改善电阻率起到很大的促进作用。
The high-temperature thermal stability of low-emissivity (Low-E) films hasimportant theoretical significance and practical worth, but has not been investigated andcharacterized systematically. F-doped SnO_2(FTO) films deposited by chemical vapordeposition (CVD) and Ag-based multilayer films deposited by magnetron sputteringmethod were studied and post-treated at high temperatures in the muffle furnace andtoughening furnace, respectively. The temperature and time effects on the structures, filmmorphologies and photoelectrical properties were investigated by X-ray diffraction (XRD),field emission scanning electron microscope (FESEM), atomic force microscope (AFM),UV-Vis spectrophotometer and physical property measurement system (PPMS). Theroom-temperature photoluminescence (PL) mechanism of FTO films were studied withthe micro-Raman Spectroscopy. The element distribution in the films has been researchedby X-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy (AES) andthe conductive mechanism has been discussed. The specific research contents are asfollows:
FTO films with SnO_2:F/SiO_xCystructure possess good high-temperature thermalstability, the temperature resistance can be improved to600℃and the longest time is15min. When the temperaute and time are higher or longer than this condition, the opticaland electrical properties of FTO films become deteriorative. The main component in thefilm interior is non-stoichiometric SnO_(2-x):F (x≈0.8~0.9) with polycrystalline cassiteritetetragonal crystal structure and the most obvious preferred orientation of (200) plane, Fatoms occupy the substitutional positions in SnO_2lattice. The room temperaturephotoluminescence spectra of FTO films can be divided into three parts in the region of325~650nm. The ultraviolet emission is attributed to a recombination of photogeneratedelectrons with the holes. The violet emission at385.20nm is related with the fluorinesubstitutions, while the violet emissions at409.33nm and441.69nm belong to oxygenvacancies with a positive chargeV
O and with two positive chargesV
O, respectively.The bluegreen emission is related with the surface states and structural defects. The [O]/[Sn] ratio in the film interior has been less effected by tempering temperature andtime and has little contribution to the deterioration of conductivity. With the increasingtemperature and time, the relative content of oxygen vacancies at the surface layerdecreases, the diffusion and lattice distortion between FTO layer and SiO_xCylayerbecome more severe, which is in good agreement with the increase of film resistivity.
Compared with the Ag-based films with glass/TiO_2/ZnO/Ag/NiCrO_x/SnO_2/Si_3N_4multilayer structure, when pre-deposited1.1nm NiCrO_xand12nm Si_3N_4under Ag layer,the modified Ag-based films with glass/Si_3N_4/TiO_2/NiCrO_x/ZnO/Ag/NiCrO_x/SnO_2/Si_3N_4multilayer structure possess better thermal stability and the highest temperature resistancecan be improved to600℃. When the modified Ag-based films are treated at60±1℃withthe humidity of90±2%, the water resistence has been improved to17days. The multilayerfilms contain a crystalline Ag layer with3C structure and amorphous layers. Atransformation of the preferred orientation from (111) plane to (220) plane occurs whenthe temperature is higher than600°C. When the modified Ag-based films were temperedat675±25℃for6min in the toughening furnace, some amount of Ag2O exists in Ag layer.The ratio of the relative content of CrIbonded with oxygen and CrIIin amorphous states inthe under NiCrO_xlayer increases from0.62to0.74after tempered for6min, whichindicates the oxidization of Ag layer may be resulted from the diffusion from the underlayers. The improved compactness and crystallinity of the functional Ag layer aftertempering play a positive role in decreasing the film resistivity.
引文
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