摘要
作为一种拥有解决全球能源短缺和治理环境污染的潜在能力，半导体光催化剂已经引起了非常广泛的关注。而开发高效稳定的可见光光催化剂已经成为光催化领域研究的热点。半导体实现可见光响应的前提是带隙与太阳光谱中可见光区域相匹配，而获得高效稳定光催化剂的基础是提高半导体光催化剂的光生载流子分离效率和可回收利用率。本文围绕新型可见光光催化剂BiOI和B2WO6粉体高的载流子复合率和回收成本的现况，设计制备了具有高光催化活性和强回收再利用能力的BiOI/Bi2WO6基（复合）可见光光催化剂。用光催化剂降解污染物的同时，也深刻体会到污染治理之不易，所以本文还初步研究了用于节能环保型白光发光二极管（WLED）灯用K2SiF6: Mn4+红色荧光粉。具体的研究内容和已取得的研究成果如下：
（1）用乙二醇做溶剂，采用溶剂热法通过调整前驱体中Bi/I的比值为1:1，1:1.5，1:2，1:3和1:5，制备了一系列晶型由Bi7O9I3到BiOI持续变化的样品。通过XRD，TG等测试手段确认了Bi7O9I3样品的晶体结构。获得的Bi7O9I3样品具有空心分层结构的三维自组装形貌和高达68.86m2·g的比表面积，再结合晶体沿光催化活性（110）晶面的择优生长使Bi7O9I3拥有优异的光催化降解特性。另外，通过在Bi7O9I3的制备过程中添加微量水来调控Bi7O9I3的微观形貌，从而制备了一系列光催化性能更强的不同形貌的Bi7O9I3样品，XRD谱和SEM照片显示微量水没有改变Bi7O9I3的晶型，而微结构由原来的空心球状变成了更加开放的三维分层结构。光催化降解实验表明添加微量水后的全部样品都拥有比空心分层球体Bi7O9I3更强的光催化性能。
（2）通过静电纺丝和溶剂热法的结合，成功制备了BiOI薄片在TiO2纳米纤维表面的可控合成，得到TiO2@BiOI复合膜，通过调整反应时间和BiOI前驱体的初始浓度可以方便的调控TiO2纤维表面上BiOI的尺寸，形貌和密度，进而改善光催化性能。TiO2@BiOI复合膜在可见光照射下具有优异的光催化性能，同时复合膜具有更高的固液分离能力，方便反应完成后的回收再利用。通过研究复合薄膜的光致发光，瞬态光电流响应曲线和XPS谱证明了在TiO2和BiOI接触界面形成了可降低区域内光生电子空穴对复合概率的异质结，从而提高光催化活性。为了进一步改善TiO2@BiOI薄膜的力学性能，结合静电纺丝，浸泡法和溶剂热法，制备了SiO2@TiO2@BiOI的复合纤维薄膜，结果显示BiOI在SiO2@TiO2表面生长的形貌类似于TiO2@BiOI。SiO2@TiO2@BiOI复合薄膜显示出强的可见光光催化性能的同时，还具有SiO2基质材料的柔韧性，可以直接通过过滤的方式光催化降解水体有机污染物。
（3）结合静电纺丝和溶剂热法成功实现了Bi2WO6薄片在SiO2纳米纤维表面的可控生长，通过Bi2WO6前驱体浓度的控制可以方便的调控SiO2纳米纤维表面Bi2WO6的形貌和密度。在复合膜中，Bi2WO6被分散固定在SiO2纳米纤维的表面，这种结构有效防止了Bi2WO6在光催化反应过程中的团聚，并赋予了Bi2WO6新的光催化反应方式，比如复合膜较好的拉伸强度和弹性模量可以使膜直接通过过滤的形式降解有机污染物，同时极大的改善了Bi2WO6光催化剂的回收再利用能力。通过测试薄膜热处理前后的XRD，SEM和力学性能，发现Bi2WO6@SiO2复合纤维具有优异的热稳定性和拉伸强度，另外，SiO2@Bi2WO6复合薄膜可以在需要热处理的情况下保护Bi2WO6在高温时避免发生团聚。改善了光催化剂的回收再利用能力后，为了进一步优化SiO2@Bi2WO6的光催化活性，通过结合静电纺丝、浸泡法和溶剂热法设计和制备了SiO2@TiO2@Bi2WO6核-核-壳结构的复合纤维，测试结果显示，与SiO2@Bi2WO6不同，长在TiO2包覆层表面的Bi2WO6的形貌更小更分散，光催化活性也远大于SiO2@Bi2WO6薄膜，同时还继承了SiO2@Bi2WO6复合膜的柔韧性。
（4）以廉价的SiO2粉末为硅源，在HF/KMnO4水溶液中用简单的氧化还原反应制备了高亮度的K2SiF6: Mn4+红色荧光粉，制备的粉体的量子效率为74%。通过荧光粉的SEM，XRD和PL图谱的测试结果表明K2SiF6: Mn4+具有作为节能环保型暖白光LED用红色荧光粉的形貌和发光特性。LED的封装实验显示混合K2SiF6: Mn4+和商用YAG: Ce荧光粉可以获得3510K暖白光色温，90.9高显色指数和81.56lm/W发光效率的暖白光LED。K2SiF6: Mn4+红色荧光粉优异的光学性能和低成本高效率的制造方法使其在暖白光LED领域具有的巨大的应用潜力。
Semiconductor photocatalysis has received much attention as a potential solution to theworldwide energy shortage and counteracting environmental degradation. Visible-light-drivenphotocatalysts with high activity and stability had attracted a great deal of attention. It wasnecessary to make the band gap of photocatalysts match with that of the solar energy and toexploit way to enhance the photo-generated electron-hole separation. In this paper, in view ofthe market demand, the BiOI/Bi2WO6-base visible light photocatalysts with excellentphtocatalytic activity and recycling was designed. Meanwhile, Synthesis of K2SiF6: Mn4+phosphor and their application in warm-white LED
(1) A series of crystal continuously changing from Bi7O9I3to BiOI were successfullyfabricated using an ethylene glycol-assisted solvothermal process by adjusting theconcentration of precursor with different I/Bi molar ratios of1,1.5,2,3, and5. The productcan be determined as Bi7O9I3, based on the results of X-ray diffraction and thermogravimetryanalysis. Bi7O9I3uniform flowerlike hollow microspheres with a hole in its shell have beenobtained with larger BET specific surface area (68.86m2·g). The special structural feature ofthe hollow Bi7O9I3microsphere structure and crystal had special anisotropic growth along the(110) plane lead to high photocatalytic activity under visible light irradiation. In addition, themicro-structure of Bi7O9I3is regulated by adding a small amout of water duing preparation.All samples on the degradation of RhB under visible light irradiation exhibited higherphotocatalytic activity than that of hollow Bi7O9I3microsphere structure.
(2) Electrospinning-derived TiO2nanofibers of anatase phase were decorated with BiOInanosheets, constructing TiO2@BiOI composite fibers. Size, morphology, together withpopulation density of the BiOI nanosheets can be readily adjusted by controlling the initialconcentration of Bi(NO3)3and incubation time in the hydrothermal reaction. Compared withpristine TiO2nanofibers, the TiO2@BiOI composite fibers exhibit faster decomposition ofRhB under visible light irradiation, and meanwhile possess high separation convenience inwater purification. Photoluminescence and transient photocurrent response results evidencethe formation of p-n junction at the interface of TiO2and BiOI, which contributes a lot inpromoting the photocatalytic performance of TiO2@BiOI fibers through enhanced separation efficiency of photogenerated charge carriers. In addition, the TiO2@BiOI fibers alsodemonstrate excellent chemical stability, making their repeated reuse in water purificationfeasible. To further improve the mechanical properties of TiO2@BiOI, the SiO2@TiO2@BiOIcomposite films is synthesized by combining the electrospinning technique, soaking andsolvothermal method. The results showed that the morphology of BiOI on the surface ofSiO2@TiO2similar to those on the TiO2@BiOI, meaning SiO2@TiO2@BiOI have both thephotocatalytic activity of TiO2@BiOI and flexibility of SiO2fiber.
(3) The hierarchical SiO2@Bi2WO6composite nanofibers membranes were successfullyfabricated by combining the electrospinning technique and solvothermal method. Size,morphology, together with population density of the Bi2WO6nanosheets can be readilyadjusted by controlling the initial concentration of Bi(NO3)3in the hydrothermal reaction.Bi2WO6is dispersed on the surface of SiO2fibers not only prevent agglomeration of Bi2WO6during the photocatalytic reaction but also could be recycled easily by sedimentation. X-raydiffraction, scanning electron microscope and mechanical properties of films before and afterheat treatment results evidence that the composite fibers have excellent thermal stability andtensile strength. In order to improve the photocatalytic activity of SiO2@Bi2WO6, theSiO2@TiO2@Bi2WO6composite films is synthesized by combining the electrospinningtechnique, soaking and solvothermal method. The results showed that SiO2@TiO2@Bi2WO6has excellent photocatalytic activity and flexibility.
(4) Highly bright K2SiF6: Mn4+red phosphors with a quantum efficiency of74%weresynthesized from silicon dioxide by redox reaction in HF/KMnO4solution. The opticalproperties of LEDs containing different ratios of K2SiF6: Mn4+phosphor and commercialCe3+-doped garnets(YAG-40) yellow-green phosphor were studied. A warm-white LED, withcolor temperature of3510K and color rendering index of90.9and efficacy of81.56lm/Wwas demonstrated. These prominent optical properties together with its low-cost and highefficient fabrication approach endow the as-synthesized K2SiF6: Mn4+phosphors greatpotential for commercial applications in warm-white LED.
引文
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