(1. 浙江工業(yè)大學 化工學院，杭州 310014；
2. 綠色化學合成技術國家重點實驗室培育基地，杭州 310014)
摘 要: 本文以硫酸氧鈦為原料，氫氟酸(HF)和尿素為導向劑，采用一步水熱法制備出具有(001)晶面優(yōu)勢取向的納米顆粒構筑的TiO2空心微球。采用XRD、SEM、TEM和BET等手段對微球的形貌、結構和組成進行分析表征，以亞甲基藍(MB)為模擬污水考察樣品光催化降解MB的能力。結果表明：樣品顆粒為直徑1~3 μm的空心微球，球壁由銳鈦礦相(A-TiO2)納米晶和孔隙構成，A-TiO2納米晶的晶面具有明顯的優(yōu)勢取向，以(001)為主，平均孔徑為12.90 nm，屬介孔范圍；制備過程中適量的HF可以增強A-TiO2納米晶的結晶程度，誘導(001)晶面的形成及穩(wěn)定保存下來；當制備過程中鈦與氟的摩爾比為0.40時，A-TiO2微球具有蛋黃結構，其比表面積可達21.05 m2/g，對亞甲基藍的降解率高達99.9%，表現(xiàn)出最佳的光催化活性。
關鍵字: 二氧化鈦；(001)晶面；空心微球；光催化
（1. School of Chemical Engineering, Zhejiang University of Technology, Hangzhou 310014, China;
2. State Key Breeding Base of Green Chemistry Synthesis Technology, Hangzhou 310014, China）
Abstract:Mesoporous TiO2 microspheres self-assembled by TiO2 nano-slices were fabricated by a hydrothermal approach, using TiOSO4 as precursor, HF and urea as initiating agent. The crystal phases, morphologies, microstructures, and chemical components of the microspheres were characterized by XRD, SEM, TEM, and BET. Furthermore, the photo-catalytic property of the microspheres was investigated using methylene blue solution as simulated sewage. The results show that the morphology of the sample particles is microsphere with a diameter 1-3 μm, the wall of the microsphere is constituted of anatase (A-TiO2) nano-crystallites and cavities. The crystal planes of the A-TiO2 nano-crystallite show preferential crystallographic orientation, most of them are belong to (001) plane. The average value is 12.90 nm, which can be attributed to mesoporosity. During the fabricating process, the suitable dosage of HF improves the crystallinity of A-TiO2 nano-crystallite, induces the formation of (001) crystal plane of A-TiO2 nano-crystallite, and preserves the (001) planes stably. When the mole ratio of Ti to F is 0.40, the microstructure of A-TiO2 microsphere displays egg yolk structure, its specific surface area reaches 21.05 m2/g，its photocatalytic rate to MB reaches 99.9%，and exhibits the best photocatalytic property.
Key words: titanium dioxide; (001) crystal plan; hollow microspheres; photocatalysis
