磷酸盐封接玻璃的制备与性能研究

发布时间：2018-05-06 19:58

本文选题：磷酸盐封接玻璃 + 无铅封接玻璃　；参考：《济南大学》2016年硕士论文

【摘要】：真空平板玻璃是近年来兴起的一种节能型透明、保温、隔热材料,在保温箱柜、建筑物及车、船门窗等方面应用前景广阔。真空平板玻璃是两片玻璃板在真空加热炉中经过一次封接制成的。低熔点且热膨胀系数与玻璃板相匹配的封接焊料是制备真空玻璃的重要材料。磷酸盐系统封接玻璃的熔封温度低,热膨胀系数范围较宽,可满足真空平板玻璃封接低温化的需求,更符合封接焊料无铅化的发展趋势。实验首先在设计和制备了(Na_2O-CaO-SiO_2)-P_2O_5系统玻璃的基础上,探究了P_2O_5含量以及添加B_2O_3和ZnO、Fe_2O_3、ZrOCl_2后玻璃样品结构与性能的变化规律,以寻找符合真空平板玻璃封接要求的最佳玻璃组成。研究表明在(Na_2O-CaO-SiO_2)-P_2O_5系统玻璃中,玻璃的密度随着P_2O_5摩尔含量的增加而增大,进一步减少SiO_2含量时,玻璃化学稳定性提高,但总体上仍然较差。添加不同摩尔比的B_2O_3和ZnO系列玻璃的密度、热膨胀系数随着B_2O_3/ZnO摩尔比的增大而减小,而玻璃转变温度和膨胀软化温度则升高,玻璃化学稳定性在B_2O_3/ZnO摩尔比为1/3时最佳,但依然较差,且玻璃粉末试样受热变化的特征温度逐渐升高,封接温度高于600oC,不可用于平板玻璃封接。随着Fe_2O_3对B_2O_3取代量的增加,玻璃的密度增大,而玻璃颗粒经沸水浴后质量损失减小,化学稳定性提高,热膨胀系数逐渐减小,玻璃转变温度和膨胀软化温度则是先降低后升高,均在Fe_2O_3对B_2O_3替代量为5mol%时最小,分别为402oC和450oC,玻璃粉末试样受热变化的特征温度逐渐降低,封接温度降至500oC以下。Fe_2O_3替代ZnO系列玻璃的密度、玻璃转变温度Tg及膨胀软化温度Tf随着Fe_2O_3对ZnO替代量的增加而增大,玻璃化学稳定性提高。玻璃最佳组成为:10(R2O+RO)-24.4(Al2O3+SiO_2+ZnO)-54P_2O_5-11.6Fe_2O_3。该玻璃的密度为2.93g/cm3,玻璃颗粒经沸水浴的质量损失为0.69%,热膨胀系数为8.61×10-6/oC,膨胀软化温度为465oC,封接温度范围为395oC~490oC。向玻璃中引入ZrOCl_2,玻璃颗粒经沸水浴后质量损失进一步减小,而玻璃的热性能参数和受热变化的特征温度变化不大。在ZrOCl_2添加量为2mol%时,玻璃化学稳定性最好,沸水浴后质量损失仅为0.22%,该玻璃的密度为2.96g/cm3,热膨胀系数为8.56×10-6/oC,膨胀软化温度为459oC,封接温度范围为390oC~483oC,可用于真空玻璃封接。研究结果表明,添加B_2O_3和ZnO总体使封接玻璃的性能变差,添加Fe_2O_3和ZrOCl_2总体改善了封接玻璃的性能。
[Abstract]:Vacuum flat glass is a kind of energy saving transparent, thermal insulation material, which has a broad application prospect in the field of heat preservation cabinet, building, vehicle, ship door and window and so on. Vacuum plate glass is made of two glass plates sealed in a vacuum heating furnace. Sealing solder with low melting point and matching coefficient of thermal expansion with glass plate is an important material for preparing vacuum glass. The sealing temperature of phosphate system is low and the coefficient of thermal expansion is wide. It can meet the needs of vacuum plate glass sealing at low temperature and accord with the development trend of lead-free sealing solder. On the basis of the design and preparation of NaSZ _ 2O-CaO-SiO _ 2O _ 2- P _ 2O _ 5 system glass, the changes of the structure and properties of the glass samples after the addition of B_2O_3 and ZnO-Fe _ 2O _ 3i _ 2O _ 3-ZrO _ Cl _ Cl _ 2 are studied in order to find the best glass composition which meets the requirements of vacuum plate glass sealing. The results show that the density of the glass increases with the increase of the molar content of P_2O_5 and the chemical stability of the glass increases when the content of SiO_2 is further reduced, but on the whole, the chemical stability of the glass is still poor in the case of Na2O-CaO-SiO _ 2C _ 2C _ 2O _ 5 system glass. The thermal expansion coefficient of B_2O_3 and ZnO series glasses with different molar ratio decreases with the increase of B_2O_3/ZnO molar ratio, while the glass transition temperature and swelling softening temperature increase. The chemical stability of glass is the best when the molar ratio of B_2O_3/ZnO is 1 / 3. But it is still poor, and the characteristic temperature of the change of glass powder under heating is rising gradually, and the sealing temperature is higher than 600oC, so it can not be used for plate glass sealing. With the increase of B_2O_3 substitution by Fe_2O_3, the density of glass increases, while the mass loss of glass particles decreases after boiling water bath, the chemical stability increases, the thermal expansion coefficient decreases gradually, and the glass transition temperature and swelling softening temperature decrease first and then increase. When the substitution amount of Fe_2O_3 for B_2O_3 is 5 mol%, 402oC and 450 OC, respectively, the characteristic temperature of the thermal change of glass powder samples decreases gradually, and the sealing temperature drops to the density of ZnO series glasses replaced by FeStat _ 2O _ 3 below 500oC. The glass transition temperature (TG) and the swelling softening temperature (TF) increase with the increase of the substitution amount of Fe_2O_3 for ZnO, and the chemical stability of the glass increases. The optimum composition of the glass is as follows: 1: 10 R2O RO)-24.4(Al2O3 SiO_2 ZnO- 54P\\\ {\}\\\ {\}\ {\}\ {\}\? The density of the glass is 2.93 g / cm ~ (-3). The mass loss of the glass particles through boiling water bath is 0.69, the coefficient of thermal expansion is 8.61 脳 10 ~ (-6) / oC, the swelling softening temperature is 465oC, and the sealing temperature is 395oC _ (490oC). When ZrOCl2 was introduced into the glass, the mass loss of glass particles decreased further after boiling water bath, but the thermal properties of glass and the characteristic temperature of heating change were not changed much. When the content of ZrOCl_2 is 2 mol%, the chemical stability of the glass is the best, the mass loss after boiling water bath is only 0.22. The density of the glass is 2.96 g / cm ~ (-3), the coefficient of thermal expansion is 8.56 脳 10-6 / oC, the swelling softening temperature is 459 OC, and the sealing temperature is 390oC ~ (483oC), which can be used for vacuum glass sealing. The results show that the properties of the sealant glass become worse with the addition of B_2O_3 and ZnO, and the properties of the sealing glass are improved with the addition of Fe_2O_3 and ZrOCl_2.
【学位授予单位】：济南大学
【学位级别】：硕士
【学位授予年份】：2016
【分类号】：TQ171.1

【参考文献】