ZrSiO_4@TiO_2光催化复合材料的制备与性能研究
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摘要
二氧化钛是一种应用广泛的光催化材料。具有较高光催化活性的二氧化钛是锐钛矿型二氧化钛或者锐钛矿型与金红石型二氧化钛的混晶,纯金红石型的二氧化钛一般因颗粒粗大而导致光催化活性很低,并且锐钛矿型向金红石型转变的相变温度很低。因此,提高锐钛矿型二氧化钛的高温稳定性和耐高温化学侵蚀性能是将其用于光催化陶瓷的关键。本文采用水热法合成锐钛矿型TiO_2纳米粉体和多孔ZrSiO_4超细粉体,通过植酸改性自组装将二者复合,制备了ZrSiO_4 @TiO_2光催化复合材料,进而制备了光催化陶瓷。利用XRD、SEM、TEM、DSC、DLS、XPS和BET等手段对产物进行分析,并用在紫外光下降解甲基橙水溶液的方法测试材料的光催化活性。作者还对相关机理进行了探讨。
作者首先将钛酸丁酯(TBOT)在二乙醇胺(DEA)的络合作用下转化为TiO_2溶胶,研究了水热处理温度和保温时间对TiO_2结晶、TiO_2粒径分布、分散性等的影响。在TiO_2溶胶中添加硅酸乙酯(TEOS)再经水热处理形成了TiO_2和无定形SiO_2在纳米尺度上均匀的混合粉体。TiO_2因SiO_2的空间位阻作用抑制了颗粒长大和相变,TiO_2/SiO_2摩尔比为1的复合材料经1200℃处理2h后仍能保持锐钛矿型二氧化钛。经过高温处理的TiO_2-SiO_2复合粉体的光催化活性远高于相同条件热处理的商品锐钛矿型TiO_2 (P25)。
以氧氯化锆和硅酸乙酯为原料,氟化钠为矿化剂制备了多孔ZrSiO_4超细粉体。发现ZrSiO_4结晶度随NaF添加量和水热温度、保温时间增加而提高,但在保温一定时间后,结晶度的提高速度变慢。pH值对ZrSiO_4形貌影响较大。硅酸锆比表面积高,孔径呈双峰分布,形貌类似纳米级纤维构建的扁平的“鸟巢状”超细颗粒,形成机理可能是晶粒的第Ⅱ类聚集生长而非Ostwald熟化。
多孔ZrSiO_4的热稳定性较好。750℃处理0.5h后,晶型、显微结构和比表面积无明显变化;900℃处理0.5h后,晶型仍未改变,但纳米级锆英石纤维显著长大,导致比表面积大幅下降。多孔硅酸锆在约850℃发生放热反应,并伴随可能是水热合成时进入其晶格的氟逸出造成的少许失重。
植酸改性多孔ZrSiO_4粉体可与TiO_2纳米粉体通过自组装形成ZrSiO_4 @TiO_2复合材料,pH值影响颗粒表面电荷,为均匀包覆的关键。TiO_2不但均匀包裹ZrSiO_4的表面而且进入其狭缝中。TiO_2与ZrSiO_4结合力强,并具有良好的高温稳定性。复合粉体涂覆于釉面砖表面上经900℃的较高温度热处理10min制备牢固附着的光催化釉面砖。ZrSiO_4@TiO_2复合粉体和光催化陶瓷均具有较好的光催化性能。
实验证明了廉价的硅溶胶可取代硅酸乙酯作硅源合成多孔硅酸锆,磷酸可代替昂贵的植酸为改性剂自组装ZrSiO_4 @TiO_2光催化复合材料,以上二者均能大幅降低成本,故有利于推广应用。
Titanium dioxide is a widely used photocatalyst.The crystal phase of titanium dioxide with high photocatalytic activity is anatase titanium dioxide or the mixed crystals of anatase and rutile titanium dioxides. The photocatalytic activity of pure rutile titanium dioxide is very low, and the anatase to rutile phase transition temperature is also very low. Therefore, the key for anatase titanium dioxide to apply in photocatalytic ceramics is to improve its high temperature stability and the ability to withstand high temperature chemical attack. In this paper, anatase TiO_2 nanoparticles and porous ZrSiO_4 powder were synthesized using hydrothermal method. ZrSiO_4 @ TiO_2 photocatalytic material was prepared by self-assembling these two kinds of powders which were modified by phytic acid. The photocatalytic ceramics were prepared by the photocatalytic materials. XRD, SEM, TEM, DSC, DLS, XPS and BET were used to analyze phase composition, microstructure, partical size and relevant mechanism. The photocatalytic activities of the test materials were characterized by the method to measure degradation ratios of methyl orange solution in the UV. The relevant mechanisms have been discussed.
TiO_2 sol was prepared using tetrabutyl orthotitanate (TBOT) as starting material and diethanolamine (DEA) as chelating reagent. The effects of processing temperature and soaking time on the crystallization, particle size distribution and dispersibility of TiO_2 were investigated. Titania-silica composites were formed after adding tetraethoxysilane (TEOS) into TiO_2 sol by hydrothermal processing. The composites were uniform mixed oxides of anatase TiO_2 and amorphous SiO_2 on a nanometer scale. Titania-silica composites with 1:1 molar ratio were maintained as anatase after treatment at 1200℃for 2h because silica inhibited the transition of anatase to rutile and abnormal grain growth of titania nanocrystals. The photocatalytic activity of the composites after treatment at different temperatures was much higher than that of TiO_2 (P25) treated at the same conditions.
Porous zircon ultrafine powders were manufactured using zirconium oxychloride(ZrOCl_2), TEOS as starting materials and NaF as mineralizer. The higher content of NaF and rising temperature of hydrothermal treatment led to higher crystallinity of zircon. The increment of crystallinity of zircon decreased with the longer holding time. The morphology of zircon was greatly affected by the pH values. The porous zircon exhibited high specific surface area with a bimodal pore size distribution. Porous zircon ultrafine powders were nestle-like platelets composing of nanofibers. The synthetic mechanism of zircon porous powders was probably not Ostwald ripening but the typeⅡaggregation growth of the nanocrystals.
The porous zircon exhibited quite good high temperature stability. The crystal phase, morphology and specific surface area did not change obviously after treatment at 750℃for 0.5h. However, the crystal phase was also maintained with significant nanofiber growth and sharp reducement of specific surface area after treatment at 900℃for 0.5h. There was an obvious exothermic reaction at ca. 850℃with some weight loss because of emission of fluorine in the zircon.
ZrSiO_4 @TiO_2 composites were self-assembled using phytic acid modified porous zircon and nanotitania powders. The pH value influenced surface charges of the two kinds of particles, which played a key role in the formation of uniform TiO_2 coating on zircon powders. TiO_2 nanoparticles encapsulated ZrSiO_4 ultrafine powders uniformly and penetrated into their slits. The combination of TiO_2 and ZrSiO_4 were strong, therefore, anatase-type titania was stabilized at high temperature. Photocalytic glazed ceramic tiles were obtained by firing tiles with composites coating at moderate high temperature of 900℃for 10min. Both ZrSiO_4 @TiO_2 composites and photocatalytic ceramics showed quite good photocatalytic performance.
Cheap silica sol can replace TEOS as silica source to synthesize porous zirconium silicate. Phosphoric acid(H_3PO_4) can replace the expensive phytic acid as surface modifier to self-assemble ZrSiO_4 @TiO_2 photocatalytic composite powders. Both of them can reduce the production costs significantly and are favorable to the promotion of their application.
作者首先将钛酸丁酯(TBOT)在二乙醇胺(DEA)的络合作用下转化为TiO_2溶胶,研究了水热处理温度和保温时间对TiO_2结晶、TiO_2粒径分布、分散性等的影响。在TiO_2溶胶中添加硅酸乙酯(TEOS)再经水热处理形成了TiO_2和无定形SiO_2在纳米尺度上均匀的混合粉体。TiO_2因SiO_2的空间位阻作用抑制了颗粒长大和相变,TiO_2/SiO_2摩尔比为1的复合材料经1200℃处理2h后仍能保持锐钛矿型二氧化钛。经过高温处理的TiO_2-SiO_2复合粉体的光催化活性远高于相同条件热处理的商品锐钛矿型TiO_2 (P25)。
以氧氯化锆和硅酸乙酯为原料,氟化钠为矿化剂制备了多孔ZrSiO_4超细粉体。发现ZrSiO_4结晶度随NaF添加量和水热温度、保温时间增加而提高,但在保温一定时间后,结晶度的提高速度变慢。pH值对ZrSiO_4形貌影响较大。硅酸锆比表面积高,孔径呈双峰分布,形貌类似纳米级纤维构建的扁平的“鸟巢状”超细颗粒,形成机理可能是晶粒的第Ⅱ类聚集生长而非Ostwald熟化。
多孔ZrSiO_4的热稳定性较好。750℃处理0.5h后,晶型、显微结构和比表面积无明显变化;900℃处理0.5h后,晶型仍未改变,但纳米级锆英石纤维显著长大,导致比表面积大幅下降。多孔硅酸锆在约850℃发生放热反应,并伴随可能是水热合成时进入其晶格的氟逸出造成的少许失重。
植酸改性多孔ZrSiO_4粉体可与TiO_2纳米粉体通过自组装形成ZrSiO_4 @TiO_2复合材料,pH值影响颗粒表面电荷,为均匀包覆的关键。TiO_2不但均匀包裹ZrSiO_4的表面而且进入其狭缝中。TiO_2与ZrSiO_4结合力强,并具有良好的高温稳定性。复合粉体涂覆于釉面砖表面上经900℃的较高温度热处理10min制备牢固附着的光催化釉面砖。ZrSiO_4@TiO_2复合粉体和光催化陶瓷均具有较好的光催化性能。
实验证明了廉价的硅溶胶可取代硅酸乙酯作硅源合成多孔硅酸锆,磷酸可代替昂贵的植酸为改性剂自组装ZrSiO_4 @TiO_2光催化复合材料,以上二者均能大幅降低成本,故有利于推广应用。
Titanium dioxide is a widely used photocatalyst.The crystal phase of titanium dioxide with high photocatalytic activity is anatase titanium dioxide or the mixed crystals of anatase and rutile titanium dioxides. The photocatalytic activity of pure rutile titanium dioxide is very low, and the anatase to rutile phase transition temperature is also very low. Therefore, the key for anatase titanium dioxide to apply in photocatalytic ceramics is to improve its high temperature stability and the ability to withstand high temperature chemical attack. In this paper, anatase TiO_2 nanoparticles and porous ZrSiO_4 powder were synthesized using hydrothermal method. ZrSiO_4 @ TiO_2 photocatalytic material was prepared by self-assembling these two kinds of powders which were modified by phytic acid. The photocatalytic ceramics were prepared by the photocatalytic materials. XRD, SEM, TEM, DSC, DLS, XPS and BET were used to analyze phase composition, microstructure, partical size and relevant mechanism. The photocatalytic activities of the test materials were characterized by the method to measure degradation ratios of methyl orange solution in the UV. The relevant mechanisms have been discussed.
TiO_2 sol was prepared using tetrabutyl orthotitanate (TBOT) as starting material and diethanolamine (DEA) as chelating reagent. The effects of processing temperature and soaking time on the crystallization, particle size distribution and dispersibility of TiO_2 were investigated. Titania-silica composites were formed after adding tetraethoxysilane (TEOS) into TiO_2 sol by hydrothermal processing. The composites were uniform mixed oxides of anatase TiO_2 and amorphous SiO_2 on a nanometer scale. Titania-silica composites with 1:1 molar ratio were maintained as anatase after treatment at 1200℃for 2h because silica inhibited the transition of anatase to rutile and abnormal grain growth of titania nanocrystals. The photocatalytic activity of the composites after treatment at different temperatures was much higher than that of TiO_2 (P25) treated at the same conditions.
Porous zircon ultrafine powders were manufactured using zirconium oxychloride(ZrOCl_2), TEOS as starting materials and NaF as mineralizer. The higher content of NaF and rising temperature of hydrothermal treatment led to higher crystallinity of zircon. The increment of crystallinity of zircon decreased with the longer holding time. The morphology of zircon was greatly affected by the pH values. The porous zircon exhibited high specific surface area with a bimodal pore size distribution. Porous zircon ultrafine powders were nestle-like platelets composing of nanofibers. The synthetic mechanism of zircon porous powders was probably not Ostwald ripening but the typeⅡaggregation growth of the nanocrystals.
The porous zircon exhibited quite good high temperature stability. The crystal phase, morphology and specific surface area did not change obviously after treatment at 750℃for 0.5h. However, the crystal phase was also maintained with significant nanofiber growth and sharp reducement of specific surface area after treatment at 900℃for 0.5h. There was an obvious exothermic reaction at ca. 850℃with some weight loss because of emission of fluorine in the zircon.
ZrSiO_4 @TiO_2 composites were self-assembled using phytic acid modified porous zircon and nanotitania powders. The pH value influenced surface charges of the two kinds of particles, which played a key role in the formation of uniform TiO_2 coating on zircon powders. TiO_2 nanoparticles encapsulated ZrSiO_4 ultrafine powders uniformly and penetrated into their slits. The combination of TiO_2 and ZrSiO_4 were strong, therefore, anatase-type titania was stabilized at high temperature. Photocalytic glazed ceramic tiles were obtained by firing tiles with composites coating at moderate high temperature of 900℃for 10min. Both ZrSiO_4 @TiO_2 composites and photocatalytic ceramics showed quite good photocatalytic performance.
Cheap silica sol can replace TEOS as silica source to synthesize porous zirconium silicate. Phosphoric acid(H_3PO_4) can replace the expensive phytic acid as surface modifier to self-assemble ZrSiO_4 @TiO_2 photocatalytic composite powders. Both of them can reduce the production costs significantly and are favorable to the promotion of their application.
引文
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