钒酸盐纳米发光材料和钛酸铋系光催化薄膜的制备及性能研究
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摘要
论文分为两部分。第一部分是钒酸盐纳米材料的制备、表征及发光性能研究，这是我们研究的主要内容；第二部分是钛酸铋系薄膜的制备、表征及光催化性能研究。
发光材料是重要的功能材料之一，在照明、显示、荧光探测、光电器件等领域有着广泛的应用。随着纳米技术的迅速发展，纳米发光材料由于显示出许多体块材料所不可比拟的新的光学特性而成为人们关注和研究的热点。钒酸盐具有良好的化学稳定性和热稳定性，但对其荧光性能的研究相对较少，在本论文中，我们采用不同的合成方法制备了钒酸盐纳米发光材料，并系统地研究了其发光性质，以寻求具有高性能的新型发光材料。
在第一章中，我们简单阐述了固体发光理论，对纳米材料的基本性质、纳米发光材料的制备方法、纳米发光材料的特性进行了简要介绍，并对钒酸盐发光材料的研究概况进行了总结。
随着新型平板显示器的发展，要求具有更高发光效率、更纯发光颜色的发光材料，以稀土钒酸盐为基质的发光材料性能优良，因而引起人们较大的研究兴趣。在第二章中，我们采用沉淀法、燃烧法制备了以稀土钒酸盐(YVO_4、LaVO_4)为基质的纳米发光材料，并研究了其发光性质。①首次采用柠檬酸为燃料／还原剂、硝酸盐为氧化剂的溶胶-凝胶燃烧法成功制备了不同尺寸的YVO_4：Eu~(3+)纳米晶，并系统研究了制备参数，如退火温度、柠檬酸／硝酸盐的摩尔比及硝酸锂添加剂的量，对YVO_4：5mol％Eu~(3+)纳米颗粒发光性质的影响。研究表明，YVO_4：Eu~(3+)纳米晶的发光强度随退火温度的升高而升高，这表明在纳米尺寸范围内高的退火温度对发光强度是有利的；柠檬酸／硝酸盐的摩尔比是影响YVO_4：Eu~(3+)纳米晶的颗粒特征、发光强度的一个重要因素，获得最高发光强度的摩尔配比是5／2；共掺杂Li~+可以大大提高YVO_4：Eu~(3+)纳米晶的发光强度，同不加入Li~+的样品相比，加入5mol％Li~+的样品的发光强度增加了11倍。②采用沉淀法制备了YVO_4：Er~(3+)和YVO_4：Er~(3+)，Mn~(2+)纳米晶，研究表明，由于浓度猝灭的影响，当Er~(3+)掺杂浓度为0.3mol％时，YVO_4：Er~(3+)样品553nm主发光峰的发光强度最强；随着退火温度的升高，颗粒的结晶度越来越好，YVO_4：Er_(0.003)~(3+)样品的发光强度越来越高；由于从Mn~(2+)到Er~(3+)存在着有效的能量传递，使得YVO_4：Er_(0.003)~(3+)，Mn_(0.001)~(2+)样品的发光强度是YVO_4：Er_(0.003)~(3+)发光强度的1.5倍。③采用沉淀法制备了不同形貌及尺寸的LaVO_4：Eu~(3+)纳米晶，研究表明：反应pH值是影响LaVO_4：Eu~(3+)纳米晶的形貌及颗粒尺寸的重要因素，而形貌及颗粒尺寸的差异又导致LaVO_4：Eu~(3+)纳米晶发光强度的不同；在LaVO_4：Eu~(3+)纳米晶中，Eu~(3+)的荧光猝灭浓度为3mol％；由于存在Eu~(3+)→Dy~(3+)非辐射能量传递，在LaVO_4：Eu~(3+)纳米晶中共掺进Dy~(3+)后，Eu~(3+)的发光强度反而降低了。
随着应用领域的增多，对荧光粉体的需求量也急剧增加，而以各种稀土材料为基质的荧光粉体的成本较高，这就需要寻找相对低廉的新材料来代替它们。由于碱土金属钒酸盐热稳定性高、结晶性和可见光透过性好，因此有可能是一种比较合适的发光基质。在第三章中，首次采用柠檬酸溶胶-凝胶燃烧法成功制备了以碱土钒酸盐(Ca_3(VO_4)_2、Sr_3(VO_4)_2)为基质的纳米发光材料并研究了其发光特性。对于Ca_3(VO_4)_2：Eu~(3+)发光材料，最佳退火温度是750℃，此温度下制备的Ca_3(VO_4)_2：Eu~(3+)的发光强度略大于同样的合成条件下制备的稀土钒酸盐YVO_4：Eu~(3+)的发光强度；在Ca_3(VO_4)_2基质中，Eu~(3+)的猝灭浓度为6mol％；当共掺Mn~(2+)时，由于存在Eu~(3+)→Mn~(2+)的能量传递，Eu~(3+)在Ca_3(VO_4)_2基质中的发光强度急剧降低。对于Sr_3(VO_4)_2：Eu~(3+)发光材料，由于高的退火温度导致颗粒的团聚，Sr_3(VO_4)2：Eu~(3+)的发光强度随退火温度的升高而降低；柠檬酸／硝酸盐的摩尔比是影响Sr_3(VO_4)_2：Eu~(3+)的颗粒特征、发光强度的一个重要因素，获得最高发光强度的摩尔配比是6／3；加入适量的硼酸助熔剂可以提高Sr_3(VO_4)_2：Eu~(3+)的发光强度，同不加入硼酸的样品相比，加入5mol％硼酸时所制备样品的发光强度增加了1.5倍。
由于材料的性能与形貌有很大的关系，因此设计能对材料的形貌进行控制的合成方法一直是材料研究领域的重要课题。在第四章中，我们首次采用表面活性剂辅助的水溶液法制备了长棒状、近圆球状等不同形貌及大小的Pb_5(VO_4)_3OH纳米晶并对其形成机理和发光特性进行了研究。由于阴离子表面活性剂十二烷基苯磺酸钠(SDBS)和阳离子表面活性剂十二烷基二甲基苄基溴化铵(DDBAB)在溶液中所形成胶团的形状和大小、所带电荷及立体化学性质不同，造成在添加不同表面活性剂的溶液中所形成纳米晶的形貌及大小不同。Pb_5(VO_4)_3OH样品位于601nm处的发光峰来源于铅离子的~3P_1-~1S_0跃迁，而且晶粒的形态和大小影响到样品的发光效率。
在环境污染治理技术中，可以利用太阳能降解有机污染物的半导体光催化技术被认为是净化环境的技术革命。随着全球性的环境污染日趋严重，开发新型半导体光催化剂和光催化剂的固载问题日益成为人们的研究热点。在第五章中，我们选择钛酸铋系氧化物(Bi_(12)TiO_(20)、Bi_4Ti_3O_(12)、Bi_2Ti_2O_7)为研究对象，采用化学溶液分解法(CSD)制备了钛酸铋系列薄膜并研究了其光催化性能。①首次采用CSD法制备了具有高光催化活性的软铋矿型Bi_(12)TiO_(20)薄膜。研究表明，500℃退火15分钟制备的涂膜层数为4的Bi_(12)TiO_(20)薄膜光催化活性最高，紫外光照射2h后，其对甲基橙的降解率就高达94％。此外，CSD法制备的Bi_(12)TiO_(20)薄膜具有较好的抗失活稳定性，且在载玻片上附着性良好，显示出极好的应用前景。②制备了铋系层状钙钛矿型Bi_4Ti_3O_(12)和(Bi_(1-x)La_x)_4Ti_3O_(12)薄膜，并首次系统研究了其光催化性能。研究表明，550℃退火15分钟制备的4层Bi_4Ti_3O_(12)薄膜光催化活性最高。La~(3+)掺杂可以提高Bi_4Ti_3O_(12)光催化薄膜的活性，La~(3+)的最佳掺杂浓度是20at％。紫外光照射2h后，(Bi_(0.8)La_(0.2))_4Ti_3O_(12)薄膜对甲基橙的降解率为83％。另外，XRD和AFM结果显示La~(3+)在(Bi_(1-x)La_x)_4Ti_3O_(12)薄膜的退火过程中起到晶粒生长抑制剂的作用。③制备了烧绿石型Bi_2Ti_2O_7薄膜和La掺杂的钛酸铋(BLT)薄膜，并首次系统研究了它的光催化性能。研究表明，550℃退火30分钟制备的6层Bi_2Ti_2O_7薄膜光催化活性最高；La~(3+)掺杂能促进钛酸铋从烧绿石相到层状钙钛矿相的相转变，因此La~(3+)可被认为是层状钙钛矿相的稳定剂；La~(3+)掺杂可以提高Bi_2Ti_2O_7光催化薄膜的活性，La~(3+)的最佳掺杂浓度是5at％，紫外光照射2h后，BLT薄膜对甲基橙的降解率为61％。另外，XRD和AFM结果显示La~(3+)在BLT薄膜的退火过程中也起到晶粒生长抑制剂的作用。
在第六章中，我们对本论文的工作进行了总结。
This dissertation includes two parts. The first part involves the studies on preparation, characterization and photoluminescence performance of Vanadate Nanomaterials. This is the main content of this dissertation. The second part is focused on the studies on preparation, characterization and photo-catalytic performance of bismuth titanate series thin films.
Luminescence materials have found wide applications in many fields, such as display, illumination and photo-electronic devices. With the rapid development of nanotechnology, nanoscaled luminescence materials have drawn much attention and been the hot topic because these materials have many miraculous properties compared with the bulk materials. Vanadates have excellent thermal and chemical stability. Their luminescence properties, however, have not drawn enough attention. In order to explore novel luminescence systems with high efficiency, in this thesis, we synthesized vanadate nanomaterials via different methods and studied their luminescence properties systemically.
In Chapter 1, we briefly illustrated the corresponding luminescence theory of solids, the preparation methods and the unique properties of nanomaterials and nanosized luminescence materials. The research progress in the field of nanosized vanadate luminescence materials was also summarized.
In Chapter 2, we studied the synthesis and characterization of nanosized rare earth vanadate (YVO_4 and LaVO_4) luminescence materials. (1)YVO_4: Eu~(3+) nanocrystals with different sizes have been synthesized via a citric acid sol-gel combustion method using citric acid as a fuel/reductant and nitrates as oxidants. Their PL properties have been also systematically studied. The influence of processing conditions, such as the calcination temperature, the citric acid/nitrates molar ratio and the amounts of lithium nitrate (LiNO_3) additive, on the powder characteristics and fluorescence properties of the resultant yttrium orthvanadate doped with 5mol% Eu~(3+) have been investigated. From the results, we can conclude: The emission intensity of Eu~(3+) in YVO_4: Eu~(3+) increases with the increasing of the calcination temperature (T), which shows that high calcination temperature is favorable for high luminescence intensity of the samples within nanometer scale. The citric acid/nitrates ratio (9) is a predominant factor for the growth of YVO_4: Eu~(3+) nanocrystals with different particles sizes, which affects their PL emission intensity greatly. The optimumφis 5/2 for the highest luminescence intensity. The luminescence intensity of this compound is enhanced remarkably by the incorporation of Li~+ ions. The luminescence intensity of YVO_4: Eu~(3+) with addition of 5mol% Li~+ ions increases as much as 11 times compared with the Li~+ ions-free YVO_4: Eu~(3+) sample. (2)YVO_4: Er~(3+) and YVO_4: Er~(3+), Mn~(2+) nanocrystals have been synthesized by precipitation means and the luminescence properties have been investigated systematically. The following conclusions can be obtained from our study: The emission intensity of Er~(3+)in the YVO_4 host at 553 nm can reach the optimum value when the concentration of Er~(3+)is 0.3 mol%, which is a result of concentration quenching. The crystallinity of YVO_4 particles improves gradually with increasing the annealing temperature, which leads to the increasing of the PL intensity of YVO_4: Er~(3+)o.oo3 samples. As the energy transfer from Mn~(2+) to Er~(3+) exists, the PL intensity of YVO_4: Er~(3+)_(0.003), Mn~(2+)_(0.001) is about 1.5 times of that of YVO_4:Er~(3+)_(0.003) (3) LaVO_4:Eu~(3+) nanocrystals with different sizes and morphologies have been synthesized via a precipitation method. The PL properties have also been systematically studied. From the results, we can conclude: The reaction pH is a predominant influencing factor for the growth of LaVO_4: Eu~(3+) nanocrystals with different sizes and morphologies, and their sizes and morphologies affect their PL emission intensities evidently. The emission intensity is highly dependent on the dopant concentration and the optimum concentration of dopant is 3mol%. The emission intensity of Eu~(3+) in LaVO_4 matrix is lowered after co-doped with Dy~(3+) due to the energy transfer from Eu~(3+) to Dy~(3+).
In Chapter 3, we studied the combustion synthesis and characterization of nanosized alkaline earth vanadate (Ca_3(VO_4)_2 and Sr_3(VO_4)_2) luminescence materials. Ca_3(VO_4)_2:Eu~(3+), Mn~(2+) powders with different sizes and morphologies have been synthesized via a citric acid sol-gel combustion method using citric acid as a fuel/reductant and nitrates as oxidants. The PL properties have been also systematically studied. The optimized annealing temperature is 750℃in the present case. The emission intensity at 613 nm of Eu~(3+) in the Ca_3(VO_4)_2 host can reach the optimum value when the concentration of Eu~(3+) is 6 mol%, because of the existence of concentration quenching. The emission intensity of Ca_3(VO_4)_2: Eu~(3+), Mn~(2+) decreases owing to the energy transfer from Eu~(3+) to Mn~(2+). Sr_3(VO_4)_2: Eu~(3+) nanocrystals with different sizes and morphologies have also been synthesized via a citric acid combustion method. The effects of processing parameters, such as the molar ratio of citric acid to nitrates (φ), calcination temperature (T) and the amounts of the additive boric acid HBO_3 (B) on the powder characteristics and fluorescence properties of the resultant Sr_3(VO_4)_2 doped with 5% Eu~(3+) have been investigated. From the results, we can conclude: The molar ratio of citric acid to nitrates (φ) is a predominant influencing factor for the growth of Sr_3(VO_4)_2: Eu~(3+) nanocrystals with different particle sizes and emission intensities evidently. The optimumφis 6/3 for the highest luminescence intensity. The emission intensity of Sr_3(VO_4)_2 : Eu~(3+) decreases with the increasing of the calcination temperature (T), owing to the falling of the specific surface areas. The optimum addition amount of boric acid is 5 mol% of the total reagent. The emission intensity of Sr_3(VO_4)_2: Eu~(3+) increases 1.5 times compared with the particles prepared without the additive.
In Chapter 4, rod-like or spherical Pb_5(VO_4)_3OH nanocrystals have been successfully prepared through a precipitation process in the presence of sodium dodecylbenzenesulfonate (SDBS) or dodecyldimethylbenzylammonium bromide (DDBAB), respectively. The effect of ion-surfactants in the formation process of nanocrystals may be correlated with the charge and stereochemistry properties of the surfactants. The 601 nm emission of the Pb_5(VO_4)_3OH nanocrystals is ascribed to the ~3P_1-~1S_0 transition of Pb~(2+) ions.
As one of the novel pollutant treatment method, photocatalysis gains more and more attentions in the field of environmental purification. Developing new photocatalysts and the supported technique of photocatalysts have always been the hot topic of the researchers. In Chapter 5, we chose bismuth titanate (Bi_(12)TiO_(20) Bi_4Ti_3O_(12) and Bi_2Ti_2O_7) as the study target, prepared bismuth titanate series thin films by CSD(chemical solution decomposition) method and systematically examined their photocatalytic performance. (1)Sillenite Bi_(12)TiO_(20) thin films with high photocatalytic activity have been firstly prepared. When annealed at 500℃for 15 minutes, the prepared sample with 4 coatings exhibits the highest photocatalytic activity. After irradiation for 2 h, the methyl orange solution is degraded by 94% on the Bi_(12)TiO_(20) thin films annealed at 500℃for 15 minutes. Moreover, Bi_(12)TiO_(20) thin films prepared by CSD method show a good anti-inactivation stability and adhere well on the silicate substrate after they have been used for many times. (2)Bi_4Ti_3O_(12) and (Bi_(1-x)La_x)_4Ti_3O_(12) with bismuth-layered perovskite structure thin films were successfully prepared and their photocatalytic properties have been firstly investigated. When annealed at 550℃for 15 minutes, the prepared Bi_4Ti_3O_(12) thin films by 4 coating cycles exhibited the highest photocatalytic activity. La~(3+) doping could improve the photocatalytic activity of Bi_4Ti_3O_(12) thin films. An optimal La~(3+) dopant amount for (Bi_(1-x)La_x)_4Ti_3O_(12) thin films is 20 at%. After irradiation for 2h, the methyl orange solution was degraded by 83% on the (Bi_(0.8)La_(0.2))_4Ti_3O_(12) films. Additionally, substituted La~(3+) ions can act as a grain-growth inhibitor in perovskite (Bi_(1-x)La_x)_4Ti_3O_(12) thin films. (3)Dopant-free Bi_2Ti_2O_7(BT) thin films with pyrochlore structure and La-doped bismuth titanate (BLT) thin films were successfully prepared and their photocatalytic properties were firstly investigated. When annealed at 550℃for 30 minutes, the prepared BT thin films by 6 coatings cycles exhibited the highest photocatalytic activity. La~(3+) doping could improve the photocatalytic activity of BT thin films. An optimal La~(3+) dopant amount for BLT thin films is 5 at%. After irradiation for 2 h, the methyl orange solution was degraded by 61% on the BLT films annealed at 550℃for 30 minutes. In addition, substituted La~(3+) ions can act as a stabilizer of perovskite BLT and a grain-growth inhibitor in BLT thin films.
In Chapter 6, a concise summary of our work was given.
发光材料是重要的功能材料之一，在照明、显示、荧光探测、光电器件等领域有着广泛的应用。随着纳米技术的迅速发展，纳米发光材料由于显示出许多体块材料所不可比拟的新的光学特性而成为人们关注和研究的热点。钒酸盐具有良好的化学稳定性和热稳定性，但对其荧光性能的研究相对较少，在本论文中，我们采用不同的合成方法制备了钒酸盐纳米发光材料，并系统地研究了其发光性质，以寻求具有高性能的新型发光材料。
在第一章中，我们简单阐述了固体发光理论，对纳米材料的基本性质、纳米发光材料的制备方法、纳米发光材料的特性进行了简要介绍，并对钒酸盐发光材料的研究概况进行了总结。
随着新型平板显示器的发展，要求具有更高发光效率、更纯发光颜色的发光材料，以稀土钒酸盐为基质的发光材料性能优良，因而引起人们较大的研究兴趣。在第二章中，我们采用沉淀法、燃烧法制备了以稀土钒酸盐(YVO_4、LaVO_4)为基质的纳米发光材料，并研究了其发光性质。①首次采用柠檬酸为燃料／还原剂、硝酸盐为氧化剂的溶胶-凝胶燃烧法成功制备了不同尺寸的YVO_4：Eu~(3+)纳米晶，并系统研究了制备参数，如退火温度、柠檬酸／硝酸盐的摩尔比及硝酸锂添加剂的量，对YVO_4：5mol％Eu~(3+)纳米颗粒发光性质的影响。研究表明，YVO_4：Eu~(3+)纳米晶的发光强度随退火温度的升高而升高，这表明在纳米尺寸范围内高的退火温度对发光强度是有利的；柠檬酸／硝酸盐的摩尔比是影响YVO_4：Eu~(3+)纳米晶的颗粒特征、发光强度的一个重要因素，获得最高发光强度的摩尔配比是5／2；共掺杂Li~+可以大大提高YVO_4：Eu~(3+)纳米晶的发光强度，同不加入Li~+的样品相比，加入5mol％Li~+的样品的发光强度增加了11倍。②采用沉淀法制备了YVO_4：Er~(3+)和YVO_4：Er~(3+)，Mn~(2+)纳米晶，研究表明，由于浓度猝灭的影响，当Er~(3+)掺杂浓度为0.3mol％时，YVO_4：Er~(3+)样品553nm主发光峰的发光强度最强；随着退火温度的升高，颗粒的结晶度越来越好，YVO_4：Er_(0.003)~(3+)样品的发光强度越来越高；由于从Mn~(2+)到Er~(3+)存在着有效的能量传递，使得YVO_4：Er_(0.003)~(3+)，Mn_(0.001)~(2+)样品的发光强度是YVO_4：Er_(0.003)~(3+)发光强度的1.5倍。③采用沉淀法制备了不同形貌及尺寸的LaVO_4：Eu~(3+)纳米晶，研究表明：反应pH值是影响LaVO_4：Eu~(3+)纳米晶的形貌及颗粒尺寸的重要因素，而形貌及颗粒尺寸的差异又导致LaVO_4：Eu~(3+)纳米晶发光强度的不同；在LaVO_4：Eu~(3+)纳米晶中，Eu~(3+)的荧光猝灭浓度为3mol％；由于存在Eu~(3+)→Dy~(3+)非辐射能量传递，在LaVO_4：Eu~(3+)纳米晶中共掺进Dy~(3+)后，Eu~(3+)的发光强度反而降低了。
随着应用领域的增多，对荧光粉体的需求量也急剧增加，而以各种稀土材料为基质的荧光粉体的成本较高，这就需要寻找相对低廉的新材料来代替它们。由于碱土金属钒酸盐热稳定性高、结晶性和可见光透过性好，因此有可能是一种比较合适的发光基质。在第三章中，首次采用柠檬酸溶胶-凝胶燃烧法成功制备了以碱土钒酸盐(Ca_3(VO_4)_2、Sr_3(VO_4)_2)为基质的纳米发光材料并研究了其发光特性。对于Ca_3(VO_4)_2：Eu~(3+)发光材料，最佳退火温度是750℃，此温度下制备的Ca_3(VO_4)_2：Eu~(3+)的发光强度略大于同样的合成条件下制备的稀土钒酸盐YVO_4：Eu~(3+)的发光强度；在Ca_3(VO_4)_2基质中，Eu~(3+)的猝灭浓度为6mol％；当共掺Mn~(2+)时，由于存在Eu~(3+)→Mn~(2+)的能量传递，Eu~(3+)在Ca_3(VO_4)_2基质中的发光强度急剧降低。对于Sr_3(VO_4)_2：Eu~(3+)发光材料，由于高的退火温度导致颗粒的团聚，Sr_3(VO_4)2：Eu~(3+)的发光强度随退火温度的升高而降低；柠檬酸／硝酸盐的摩尔比是影响Sr_3(VO_4)_2：Eu~(3+)的颗粒特征、发光强度的一个重要因素，获得最高发光强度的摩尔配比是6／3；加入适量的硼酸助熔剂可以提高Sr_3(VO_4)_2：Eu~(3+)的发光强度，同不加入硼酸的样品相比，加入5mol％硼酸时所制备样品的发光强度增加了1.5倍。
由于材料的性能与形貌有很大的关系，因此设计能对材料的形貌进行控制的合成方法一直是材料研究领域的重要课题。在第四章中，我们首次采用表面活性剂辅助的水溶液法制备了长棒状、近圆球状等不同形貌及大小的Pb_5(VO_4)_3OH纳米晶并对其形成机理和发光特性进行了研究。由于阴离子表面活性剂十二烷基苯磺酸钠(SDBS)和阳离子表面活性剂十二烷基二甲基苄基溴化铵(DDBAB)在溶液中所形成胶团的形状和大小、所带电荷及立体化学性质不同，造成在添加不同表面活性剂的溶液中所形成纳米晶的形貌及大小不同。Pb_5(VO_4)_3OH样品位于601nm处的发光峰来源于铅离子的~3P_1-~1S_0跃迁，而且晶粒的形态和大小影响到样品的发光效率。
在环境污染治理技术中，可以利用太阳能降解有机污染物的半导体光催化技术被认为是净化环境的技术革命。随着全球性的环境污染日趋严重，开发新型半导体光催化剂和光催化剂的固载问题日益成为人们的研究热点。在第五章中，我们选择钛酸铋系氧化物(Bi_(12)TiO_(20)、Bi_4Ti_3O_(12)、Bi_2Ti_2O_7)为研究对象，采用化学溶液分解法(CSD)制备了钛酸铋系列薄膜并研究了其光催化性能。①首次采用CSD法制备了具有高光催化活性的软铋矿型Bi_(12)TiO_(20)薄膜。研究表明，500℃退火15分钟制备的涂膜层数为4的Bi_(12)TiO_(20)薄膜光催化活性最高，紫外光照射2h后，其对甲基橙的降解率就高达94％。此外，CSD法制备的Bi_(12)TiO_(20)薄膜具有较好的抗失活稳定性，且在载玻片上附着性良好，显示出极好的应用前景。②制备了铋系层状钙钛矿型Bi_4Ti_3O_(12)和(Bi_(1-x)La_x)_4Ti_3O_(12)薄膜，并首次系统研究了其光催化性能。研究表明，550℃退火15分钟制备的4层Bi_4Ti_3O_(12)薄膜光催化活性最高。La~(3+)掺杂可以提高Bi_4Ti_3O_(12)光催化薄膜的活性，La~(3+)的最佳掺杂浓度是20at％。紫外光照射2h后，(Bi_(0.8)La_(0.2))_4Ti_3O_(12)薄膜对甲基橙的降解率为83％。另外，XRD和AFM结果显示La~(3+)在(Bi_(1-x)La_x)_4Ti_3O_(12)薄膜的退火过程中起到晶粒生长抑制剂的作用。③制备了烧绿石型Bi_2Ti_2O_7薄膜和La掺杂的钛酸铋(BLT)薄膜，并首次系统研究了它的光催化性能。研究表明，550℃退火30分钟制备的6层Bi_2Ti_2O_7薄膜光催化活性最高；La~(3+)掺杂能促进钛酸铋从烧绿石相到层状钙钛矿相的相转变，因此La~(3+)可被认为是层状钙钛矿相的稳定剂；La~(3+)掺杂可以提高Bi_2Ti_2O_7光催化薄膜的活性，La~(3+)的最佳掺杂浓度是5at％，紫外光照射2h后，BLT薄膜对甲基橙的降解率为61％。另外，XRD和AFM结果显示La~(3+)在BLT薄膜的退火过程中也起到晶粒生长抑制剂的作用。
在第六章中，我们对本论文的工作进行了总结。
This dissertation includes two parts. The first part involves the studies on preparation, characterization and photoluminescence performance of Vanadate Nanomaterials. This is the main content of this dissertation. The second part is focused on the studies on preparation, characterization and photo-catalytic performance of bismuth titanate series thin films.
Luminescence materials have found wide applications in many fields, such as display, illumination and photo-electronic devices. With the rapid development of nanotechnology, nanoscaled luminescence materials have drawn much attention and been the hot topic because these materials have many miraculous properties compared with the bulk materials. Vanadates have excellent thermal and chemical stability. Their luminescence properties, however, have not drawn enough attention. In order to explore novel luminescence systems with high efficiency, in this thesis, we synthesized vanadate nanomaterials via different methods and studied their luminescence properties systemically.
In Chapter 1, we briefly illustrated the corresponding luminescence theory of solids, the preparation methods and the unique properties of nanomaterials and nanosized luminescence materials. The research progress in the field of nanosized vanadate luminescence materials was also summarized.
In Chapter 2, we studied the synthesis and characterization of nanosized rare earth vanadate (YVO_4 and LaVO_4) luminescence materials. (1)YVO_4: Eu~(3+) nanocrystals with different sizes have been synthesized via a citric acid sol-gel combustion method using citric acid as a fuel/reductant and nitrates as oxidants. Their PL properties have been also systematically studied. The influence of processing conditions, such as the calcination temperature, the citric acid/nitrates molar ratio and the amounts of lithium nitrate (LiNO_3) additive, on the powder characteristics and fluorescence properties of the resultant yttrium orthvanadate doped with 5mol% Eu~(3+) have been investigated. From the results, we can conclude: The emission intensity of Eu~(3+) in YVO_4: Eu~(3+) increases with the increasing of the calcination temperature (T), which shows that high calcination temperature is favorable for high luminescence intensity of the samples within nanometer scale. The citric acid/nitrates ratio (9) is a predominant factor for the growth of YVO_4: Eu~(3+) nanocrystals with different particles sizes, which affects their PL emission intensity greatly. The optimumφis 5/2 for the highest luminescence intensity. The luminescence intensity of this compound is enhanced remarkably by the incorporation of Li~+ ions. The luminescence intensity of YVO_4: Eu~(3+) with addition of 5mol% Li~+ ions increases as much as 11 times compared with the Li~+ ions-free YVO_4: Eu~(3+) sample. (2)YVO_4: Er~(3+) and YVO_4: Er~(3+), Mn~(2+) nanocrystals have been synthesized by precipitation means and the luminescence properties have been investigated systematically. The following conclusions can be obtained from our study: The emission intensity of Er~(3+)in the YVO_4 host at 553 nm can reach the optimum value when the concentration of Er~(3+)is 0.3 mol%, which is a result of concentration quenching. The crystallinity of YVO_4 particles improves gradually with increasing the annealing temperature, which leads to the increasing of the PL intensity of YVO_4: Er~(3+)o.oo3 samples. As the energy transfer from Mn~(2+) to Er~(3+) exists, the PL intensity of YVO_4: Er~(3+)_(0.003), Mn~(2+)_(0.001) is about 1.5 times of that of YVO_4:Er~(3+)_(0.003) (3) LaVO_4:Eu~(3+) nanocrystals with different sizes and morphologies have been synthesized via a precipitation method. The PL properties have also been systematically studied. From the results, we can conclude: The reaction pH is a predominant influencing factor for the growth of LaVO_4: Eu~(3+) nanocrystals with different sizes and morphologies, and their sizes and morphologies affect their PL emission intensities evidently. The emission intensity is highly dependent on the dopant concentration and the optimum concentration of dopant is 3mol%. The emission intensity of Eu~(3+) in LaVO_4 matrix is lowered after co-doped with Dy~(3+) due to the energy transfer from Eu~(3+) to Dy~(3+).
In Chapter 3, we studied the combustion synthesis and characterization of nanosized alkaline earth vanadate (Ca_3(VO_4)_2 and Sr_3(VO_4)_2) luminescence materials. Ca_3(VO_4)_2:Eu~(3+), Mn~(2+) powders with different sizes and morphologies have been synthesized via a citric acid sol-gel combustion method using citric acid as a fuel/reductant and nitrates as oxidants. The PL properties have been also systematically studied. The optimized annealing temperature is 750℃in the present case. The emission intensity at 613 nm of Eu~(3+) in the Ca_3(VO_4)_2 host can reach the optimum value when the concentration of Eu~(3+) is 6 mol%, because of the existence of concentration quenching. The emission intensity of Ca_3(VO_4)_2: Eu~(3+), Mn~(2+) decreases owing to the energy transfer from Eu~(3+) to Mn~(2+). Sr_3(VO_4)_2: Eu~(3+) nanocrystals with different sizes and morphologies have also been synthesized via a citric acid combustion method. The effects of processing parameters, such as the molar ratio of citric acid to nitrates (φ), calcination temperature (T) and the amounts of the additive boric acid HBO_3 (B) on the powder characteristics and fluorescence properties of the resultant Sr_3(VO_4)_2 doped with 5% Eu~(3+) have been investigated. From the results, we can conclude: The molar ratio of citric acid to nitrates (φ) is a predominant influencing factor for the growth of Sr_3(VO_4)_2: Eu~(3+) nanocrystals with different particle sizes and emission intensities evidently. The optimumφis 6/3 for the highest luminescence intensity. The emission intensity of Sr_3(VO_4)_2 : Eu~(3+) decreases with the increasing of the calcination temperature (T), owing to the falling of the specific surface areas. The optimum addition amount of boric acid is 5 mol% of the total reagent. The emission intensity of Sr_3(VO_4)_2: Eu~(3+) increases 1.5 times compared with the particles prepared without the additive.
In Chapter 4, rod-like or spherical Pb_5(VO_4)_3OH nanocrystals have been successfully prepared through a precipitation process in the presence of sodium dodecylbenzenesulfonate (SDBS) or dodecyldimethylbenzylammonium bromide (DDBAB), respectively. The effect of ion-surfactants in the formation process of nanocrystals may be correlated with the charge and stereochemistry properties of the surfactants. The 601 nm emission of the Pb_5(VO_4)_3OH nanocrystals is ascribed to the ~3P_1-~1S_0 transition of Pb~(2+) ions.
As one of the novel pollutant treatment method, photocatalysis gains more and more attentions in the field of environmental purification. Developing new photocatalysts and the supported technique of photocatalysts have always been the hot topic of the researchers. In Chapter 5, we chose bismuth titanate (Bi_(12)TiO_(20) Bi_4Ti_3O_(12) and Bi_2Ti_2O_7) as the study target, prepared bismuth titanate series thin films by CSD(chemical solution decomposition) method and systematically examined their photocatalytic performance. (1)Sillenite Bi_(12)TiO_(20) thin films with high photocatalytic activity have been firstly prepared. When annealed at 500℃for 15 minutes, the prepared sample with 4 coatings exhibits the highest photocatalytic activity. After irradiation for 2 h, the methyl orange solution is degraded by 94% on the Bi_(12)TiO_(20) thin films annealed at 500℃for 15 minutes. Moreover, Bi_(12)TiO_(20) thin films prepared by CSD method show a good anti-inactivation stability and adhere well on the silicate substrate after they have been used for many times. (2)Bi_4Ti_3O_(12) and (Bi_(1-x)La_x)_4Ti_3O_(12) with bismuth-layered perovskite structure thin films were successfully prepared and their photocatalytic properties have been firstly investigated. When annealed at 550℃for 15 minutes, the prepared Bi_4Ti_3O_(12) thin films by 4 coating cycles exhibited the highest photocatalytic activity. La~(3+) doping could improve the photocatalytic activity of Bi_4Ti_3O_(12) thin films. An optimal La~(3+) dopant amount for (Bi_(1-x)La_x)_4Ti_3O_(12) thin films is 20 at%. After irradiation for 2h, the methyl orange solution was degraded by 83% on the (Bi_(0.8)La_(0.2))_4Ti_3O_(12) films. Additionally, substituted La~(3+) ions can act as a grain-growth inhibitor in perovskite (Bi_(1-x)La_x)_4Ti_3O_(12) thin films. (3)Dopant-free Bi_2Ti_2O_7(BT) thin films with pyrochlore structure and La-doped bismuth titanate (BLT) thin films were successfully prepared and their photocatalytic properties were firstly investigated. When annealed at 550℃for 30 minutes, the prepared BT thin films by 6 coatings cycles exhibited the highest photocatalytic activity. La~(3+) doping could improve the photocatalytic activity of BT thin films. An optimal La~(3+) dopant amount for BLT thin films is 5 at%. After irradiation for 2 h, the methyl orange solution was degraded by 61% on the BLT films annealed at 550℃for 30 minutes. In addition, substituted La~(3+) ions can act as a stabilizer of perovskite BLT and a grain-growth inhibitor in BLT thin films.
In Chapter 6, a concise summary of our work was given.
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