新型发光材料磷酸锌钾纳米片的制备

新型发光材料磷酸锌钾纳米片的制备 Synthesis of Novel Luminescent Material KZnPO 4 Nano-lamellar 马少妹 MA Shao-mei 2 first-author 王璟 WANG Jing 2 宋宝玲 SONG Bao-ling 1 廖森 LIAO Sen 1 黄增尉 HUANG Zeng-wei 2 袁爱群 YUAN Ai-qun 2 广西大学 化学化工学院,广西 南宁,530004 广西大学 化学化工学院,广西 南宁,530004 School of Chemistry and Chemical Engineering, Guangxi University School of Chemistry and Chemical Engineering, Guangxi University 广西民族大学化学化工学院 化学与生物转化过程新技术重点实验室,广西 南宁,530006 广西民族大学化学化工学院 化学与生物转化过程新技术重点实验室,广西 南宁,530006 Key Laboratory of New Technology of Chemical and Biological Transformation Processes, College of Chemistry and Chemical Engineering, Guangxi University for Nationalities Key Laboratory of New Technology of Chemical and Biological Transformation Processes, College of Chemistry and Chemical Engineering, Guangxi University for Nationalities 以ZnSO 4 ·7H 2 O和K 3 PO 4 ·3H 2 O为原料采用固相反应合成磷酸锌钾,应用均匀设计和数据挖掘技术设计实验方案,采用XRD、SEM和EDS等方法对产物进行表征,并对产物的长余辉发光性能进行了研究。结果表明,根据产物的产率和锌的含量进行回归分析可以建立2个数学模型,对模型进行优化处理可以得到固相法合成磷酸锌钾的最优工艺条件。在n(K 3 PO 4 ·3H 2 O):n(ZnSO 4 ·7H 2 O)=1.01、研磨时间31min、保温温度750℃、保温时间3.2h的最优条件下制备的KZnPO 4 纳米片,在紫外光照后可产生蓝绿色长余辉发光,最强发光峰的波长范围为415~530nm。 Potassium zinc phosphate (KZnPO 4 ) was synthesized by solid-state reaction using K 3 PO 4 ·3H 2 O and ZnSO 4 ·7H 2 O as reagents. Experimental project was designed by uniform design and data mining technology. The obtained product was characterized by X-ray diffraction, scanning electron microscope and energy disperses spectroscopy, and its property of long lasting phosphorescence was also studied. Based on the yield and zinc content, two mathematical models were established by regression analysis. The best technology conditions of synthesis can be obtained by optimization of these two models. Under the optimum reaction conditions: molar ratio of n(K 3 PO 4 ·3H 2 O):n(ZnSO 4 ·7H 2 O)=1.01, grinding time 31 min, holding temperature 750℃, holding time 3.2 h, the prepared product is KZnPO 4 with nano-lamellar structure. After ultraviolet radiation, the obtained product show blue-green long lasting phosphorescence and the highest emission peak is located at 415~530 nm. 发光材料 磷酸锌钾 数据挖掘 纳米薄片 luminescent material potassium zinc phosphate data mining technology nano-lamellar Palilla F C, A1 here A K, Tomkus M R. F1uorescence properties of alkaline earth aluminates of the type MAl2O4 activated by divalent europium [J]. Electrochem. Soc., 1968, 115(6):642-644. Song Y H, Gan S C, Deng Y F, et al. Preparation and spectral properties of β-Zn3(PO4)2:Mn2+,Ga3+ [J]. Chin. J. Lumin.(发光学报), 2006, 27(4):484-488 (in Chinese). Le S N, Navrotsky A. Energetics of phosphate frameworks containing zinc and cobalt: NaZnPO4, NaH(ZnPO4)2, NaZnPO4·H2O, NaZnPO4·4/3H2O, and NaCoem>xZn1-x PO4·4/3H2O [J]. J. Solid State Chem., 2007, 180(9):2443-2451. Harrison W T A, Gier T E, Stucky G D, et al. NaZnPO4·H2O an open-framework sodium zincophosphate with a new chiral tetrahedral framework topology [J]. Chem. Mater., 1996, 8(1):145-151. Bu X H, Thurman E G, Galen D S. A new polymorph of lithium zinc phosphate with the gristobalite-type framework topology [J]. J. Solid State Chem., 1998, 138(1):126-130. Anandalakshmi H, Sougandi I, Velavan K, et al. Single crystal EPR studies of paramagnetic ions doped zinc potassium phosphate hexahydrate:Part Ⅲ:Mn(Ⅱ)——a case of rhombic distortion [J]. Spectrochim. Acta A: Mol. Biomol. Spectrosc., 2004, 60(11):2661-2666. Ravikumar R V, Madhu N, Chandrasekhar A V, et al. Single crystal EPR and optical studies of paramagnetic ions doped zinc potassium phosphate hexahydrate——Part Ⅱ:VO(Ⅱ)——a case of substitutional site [J]. Spectrochim. Acta A:Mol. Biomol. Spectrosc., 2001, 57(14):2789-2794. Chen X, Liao S, Wang T S, et al. Knoevenagel condensation catalyzed by potassium zinc phosphate [J]. Technol. & Dev. Chem. Ind., 2008, 37(1):1-3. Zhou L, Zhou Y H, Zheng Y X, et al. Long lasting phosph0rescent properties of β-Zn3(PO4)2:Mn2+,B3+ materials [J]. Chin. J. Lumin.(发光学报), 2008, 29(6):1008-1012 (in Chinese). Liao S. Experiment Design and Data Mining Technology [M]. Beijing: Chinese Education Culture Press, 2006:11-29. Wallez G, Lucas F, Souron J P, et al. Potassium-zinc monophosphate:an original polymorphic tridymite dervate [J]. Mater. Res. Bull., 1999, 34(2):1251-1261. Garces N Y, Wang L, Bai L, et al. Role of copper in the green luminescence from ZnO crystals [J]. Appl. Phys. Lett., 2002, 81(4):622-624. 10.3788/fgxb20133401.0024 O482.31 广西科学研究与技术开发计划应用基础研究专项(桂科攻11107013-6,桂科能0992028-13)资助项目 2012-09-20 2012-11-07 2013-01-10 2020-08-11 1 34