摘要
以Al_2O_3为基质的激光材料具有硬度高,透光性与光学均匀性好,热导率高,化学成分与结构稳定等优点,目前主要有红宝石(Cr~(3+):Al_2O_3)和钛宝石(Ti:Al_2O_3)。红宝石晶体是最早和最重要的固体激光材料,作为产生可见光区域的高功率激光工作物质目前仍被广泛应用。钛宝石晶体是最佳宽带可调谐激光晶体,具有增益带宽,高饱和通量、高激光破坏阈值等特点,是综合性最好、应用最广泛的可调谐激光材料。但是单晶制作成本很高,高掺杂困难,生长单晶尺寸也受到很大限制。相对于单晶而言,透明陶瓷因为制备周期短、生产成本低、生产效率高,而且易获得大尺寸、易于加工、掺杂浓度高等优点,因此成为近年来材料领域的一个研究热点。
本文主要以Cr~(3+):Al_2O_3透明陶瓷为研究对象。研究了不同工艺制备Cr~(3+):Al_2O_3、Ti:Al_2O_3纳米粉体的性能,确定了纳米粉体最佳制备工艺条件。研究了制备工艺条件、Cr~(3+)离子掺杂浓度等对Cr~(3+):Al_2O_3透明陶瓷性能的影响。利用热重/差热分析(TG/DTA)、红外光谱(IR)、X射线衍射(XRD)、透射电镜(TEM)、扫描电镜(SEM)、电子能谱(EDS)、荧光光谱等技术对前驱物、纳米粉体及透明陶瓷进行表征。
1. Cr~(3+):Al_2O_3纳米陶瓷粉体的制备
采用共沉淀法首次制备出Cr~(3+):Al_2O_3纳米陶瓷粉体。以碳酸氢铵为沉淀剂,并与硝酸盐的混合溶液反应得到NH_4MO(OH)HCO_3 (M= Al~(3+)、Cr~(3+))前驱体,在1200℃下保温1.0h得到纯α-Al_2O_3晶相;研究分散剂、反应物初始浓度、pH值、Cr~(3+)掺杂浓度等对粉体的形貌以及发光性能的影响。(NH_4)_2SO_4的引入提高了纳米粉体的分散性,粉体颗粒分布均匀,平均粒径为58nm;样品的激发峰位于429nm和588nm,分别对应着Cr~(3+)离子~4A_2→~4T_2和~4A_2→~4T_1的能级跃迁;发射峰值位于693nm和668nm,693nm对应Cr~(3+)离子~4A_2组态间~2E_g→~4A_(2g)跃迁的R荧光谱线,而668nm为“蓝移”的另一组R线与Cr~(3+)离子~2T_(1g)→~4A_(2g)辐射跃迁的T(T_1,T_2,T_3)组荧光谱线在此处相互叠加。Cr~(3+)离子的最佳掺杂浓度为1.0wt%。
采用低温燃烧法首次制备Cr~(3+):Al_2O_3纳米粉体。研究以不同燃料(尿素、柠檬酸)制得粉体的性能。以尿素为燃料制得的粉体严重团聚。以柠檬酸为燃料(溶胶.凝胶低温燃烧法)制成的凝胶于500℃使之发生燃烧反应,再将燃烧产物于1000℃煅烧1.0h后,为α-Al_2O_3的单相氧化物粉体,乙二醇作为分散剂可提高粉体的分散性。两种不同燃料制备的纳米粉体的激发峰位于429nm和588nm,发射峰值位于693nm和668 nm。Cr~(3+)离子的最佳掺杂浓度均为1.0wt%。
2.Ti:Al_2O_3纳米陶瓷粉体的制备
采用共沉淀法、溶胶-凝胶低温燃烧法合成了Ti:Al_2O_3纳米粉体。共沉淀法制备的前驱体于1200℃煅烧1.0h得到了平均粒径小于50nm、形状为球形或类球形纯的α-Al_2O_3晶相,Ti离子掺杂浓度为2.0wt%时,也无中间相生成。溶胶-凝胶低温燃烧法制的前驱物于1000℃、保温1.0h直接得到纯的α-Al_2O_3晶相。
3.Cr~(3+):Al_2O_3透明陶瓷的制备
确定了共沉淀法制备的Cr~(3+):Al_2O_3纳米粉的烧结性能好于溶胶-凝胶低温燃烧法制备的粉体。分析了添加剂对陶瓷性能的影响:添加剂的量均应有最佳成分点,越接近该点,烧结试样性能将会越好;MgO的添加量为0.1wt%,La_2O_3的添加量为0.15wt%,Y_2O_3的添加量为0.05wt%。烧结温度和保温时间对陶瓷的微观结构、发光性能均有较大的影响,合适的烧结温度为1700℃,保温时间为10-15h。采用氢气气氛于1700℃烧结10h得到的Cr~(3+):Al_2O_3透明陶瓷的透过率在40%以上。Cr~(3+)掺杂浓度在1.25wt%,陶瓷在688nm、693nm处也具有很好的锐线荧光发射,这对激光的输出提供了可能,且实现了较高浓度的掺杂。Cr_2O_3在Cr~(3+):Al_2O_3陶瓷中主要有两个作用:①提供发光中心;②促进陶瓷烧结。
Laser media with Al_2O_3 as host materials have characteristics of high hardness, good transmittance and optical uniformity, as well as high thermal conductivity, stable chemical composition and structures. There are mainly two types of laser materials using Al_2O_3 as host materials, that is ruby (Cr~(3+):Al_2O_3) and sapphire (Ti:Al_2O_3). Ruby laser is the earliest and most important solid laser. It is still used widely in high power laser of visible wavelength. Sapphire is the optimal wide-band tunable laser crystal, and has characteristics of wide-gain, high-saturation flux and high laser damage threshold, so it is widely used as tunable laser materials. But single crystal has some restrictions, such as high-cost, low doping concentration and small size etc. Comparing with single crystal, transparent ceramics become a hot research field because of its characteristics of short producing cycle, low cost, high productivity, and transparent ceramics also possesses uniform optical property and high doping rate.
In this paper, preparation method and properties of Cr~(3+):Al_2O_3 and Ti:Al_2O_3 nano-powders were researched, the optimum parameters and the influences of fabrication parameters and doping rate of Cr~(3+) on Cr~(3+):Al_2O_3 ceramic properties were studied. The properties of precursor, nano-powders and transparent ceramics were characterized by TG/DTA, IR, XRD, TEM, SEM, EDS methods and fluorescence spectrum test.
1. Preparation of Cr~(3+):Al_2O_3 nano-powders of ceramics
Cr~(3+):Al_2O_3nano-powders was firstly prepared by co-precipitation method using NH_4HCO_3 as the precipitant. During the process, NH_4MO(OH)HCO_3 (M= Al~(3+)、Cr~(3+)) precursor was obtained , the precursor was transformed into pureα- Al_2O_3 after calcined at 1200℃for 1h. The influences of dispersant, beginning concentration of reactant, pH value, doping concentration of Cr~(3+) on the morphology and luminescence properties of powders were studied. The adding of (NH_4)_2SO_4 improved the dispersion property of the powders, the particles distributed uniformly with diameter of 58nm. The excitation peaks of the samples located at 429nm and 588nm respectively, corresponding to the transition of ~4A_2→~4T_2 and ~4A_2→~4T_1, the emission peaks are at 693nm, 668nm and 693nm respectively, corresponding to the R spectrum line of ~2E_g→~4A_(2g) transition of ~4A_2 level. Emission peak at 668nm is the superimposition of blue-shifted R line and T(T_1,T_2,T_3) spectrum line of ~2T_(1g)→~4A_(2g) transition. The optimum doping concentration of Cr~(3+) is 1.0wt%.
Cr~(3+):Al_2O_3 nano-powder was firstly synthesized by low temperature combustion method. Properties of powders by different reductive agents (urea and citric acid) were studied. Pureα-Al_2O_3 prepared by using urea as the reductive agent has severe aggregation. When using citric acid as the reductive agent, precursors can burn at 500℃and can transform into pureα- Al_2O_3 when calcined at 1000℃for 1h. The adding of polyethylene glycol as the disperser can alleviate the aggregation of the sample. The emission peak of nano-powders using former two kind of fuel are at 429nm and 588nm respectively, emission peaks are at 693nm and 668nm respectively, the optimum doping concentration of Cr~(3+) is 1.0wt%.
2. Preparation of Ti:Al_2O_3 nano-powders of ceramics
Ti:Al_2O_3 nano-powders was synthesized by co-precipitation and sol-gel low combustion methods. For co-precipitation process, when calcined at 1200℃for lh, the particle size is less than 50nm, and morphology is spherical, and there is no intermediate phase when Ti doping is 2 wt%. For sol-gel low combustion process, pureα-Al_2O_3 phase can be obtained when calcined at 1000℃for 1h.
3. Fabrication of Cr~(3+):Al_2O_3 transparent ceramics
It can be concluded that the property of samples made by co-precipitation method is better than sol-gel low temperature combustion method. The effect of addictives to the properties of ceramics was studied, the optimum conditions of the amount of addictives was analyzed. The concentration of MgO is 0.1wt%, La_2O_3 is 0.15wt%, Y_2O_3 is 0.05wt%. There are great influences of sintering temperature and time on the properties of the sample. The optimum sintering parameters is 1700℃, 10~15h. The transmittance of Cr~(3+):Al_2O_3 ceramics samples sintered at 1700℃for 10h under hydrogen atmosphere is about 40%, the sample has good luminescence property at 688nm and 693nm when the doping concentration of Cr~(3+) is 1.25wt%, and this result provides the possibility of laser oscillation and high rate of doping. The functions of Cr_2O_3 in Cr~(3+):Al_2O_3 ceramic are to provide luminescent center and improve sintering of ceramics.
引文
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