一维PZT的水热法制备及其生长机制研究

发布时间：2018-03-16 01:20

本文选题：水热法　切入点：PZT　出处：《哈尔滨工业大学》2010年硕士论文　论文类型：学位论文

【摘要】：本文以硝酸铅[Pb(NO_3)_2]/醋酸铅[Pb(CH3COOH)_2·3H_2O]、钛酸丁酯[Ti(C_4H_9O)_4]、氧氯化锆[ZrOCl_2·8H_2O]/硝酸锆[Zr(NO_3)_4·5H_2O]/硝酸氧锆[ZrO(NO_3)_2·2H_2O]为主要原料,氨水为沉淀剂,KOH为矿化剂,通过在水热体系中添加表面活性剂十六烷基三甲基溴化铵(CTAB)和聚乙烯醇(PVA1750),成功地合成了PbZr_0.52Ti_0.48O_3(PZT)一维结构。通过XRD、RAMAN、SEM和TEM对产物的物相和微观结构进行了较为系统的研究。研究结果表明,当以CTAB表面活性剂的浓度为5g/L时,制备的PZT形貌为成簇的相互垂直的棒体,其单根棒体直径约为500nm,长约8μm。在选定的反应时间(12h,24h,48h)内,随着反应时间的增加,一维结构的数量增加,其晶粒生长及形貌演化为溶解-沉淀过程。配制不同浓度的氨水,使得Zr-Ti混合液发生沉淀的PH值分别为9.5,10,10.5和11,随着PH值增大,所得PZT一维结构长径比由2变为8。TEM分析结果表明单根棒的生长取向为[001]晶向。根据实验结果分析了CTAB对PZT一维结构的作用机理,并建立了模型。以PVA1750为表面活性剂,随着其浓度由0.36g/L增大到16g/L,PZT一维结构的长径比也有所增大。当PVA1750的浓度为16g/L时,所得一维结构的直径约为300nm,长约2.5μm。Zr-Ti共沉淀体及反应产物的清洗方式对粉体形貌也有一定的的影响,两者通过离心方式清洗有利于获得分散性良好的PZT一维结构。反应时间及Zr-Ti共沉淀PH值对粉体形貌的影响与CTAB分析结果一致。KOH浓度对粉体形貌有很大的影响。当KOH浓度较低(1.48mol/L)时,其形貌为分叉生长的一维结构;而当KOH浓度较高(2mol/L)时,其形貌为围绕中心发散生长的一维结构。TEM分析结果表明单根棒的生长取向为[001]晶向。结合实验结果分析了PVA1750对PZT一维结构的作用机理,在此基础上建立了生长机理的模型。
[Abstract]:In this paper, lead nitrate [Pb(NO_3)_2] / lead acetate [Pb(CH3COOH)_2 路3H _ 2O], butyl titanate [Ti(C_4H_9O)_4], zirconium oxychloride [ZrOCl_2 路8H _ 2O] / zirconium nitrate [Zr(NO_3)_4 路5H _ 2O] / ZrO(NO_3)_2 路2H _ 2O were used as main raw materials and ammonia water as precipitator Koh as mineralizer. The one-dimensional structure of PbZr0.52TiA0.48O3PZT-1 was successfully synthesized by adding surfactant CTAB and PVA1750 in hydrothermal system. The phase and microstructure of the product were systematically studied by means of TEM and SEM. The results show that when the concentration of CTAB surfactant is 5 g / L, the morphology of PZT is a cluster of perpendicular rods with a diameter of 500 nm and a length of about 8 渭 m. Within the selected reaction time of 12 h ~ 24 h ~ (48 h), the morphology of the prepared PZT increases with the increase of reaction time. With the increase of the number of one-dimensional structure, the grain growth and morphology evolved into a dissolution-precipitation process. When different concentrations of ammonia water were prepared, the PH values of precipitation in Zr-Ti mixed solution were 9.5 ~ 1010 ~ 10.5 and 11, respectively, with the increase of PH value. The length to diameter ratio of one-dimensional PZT structure was changed from 2 to 8. Tem analysis showed that the growth orientation of single rod was [001] orientation. Based on the experimental results, the mechanism of CTAB acting on the one-dimensional structure of PZT was analyzed and the model was established. Using PVA1750 as surfactant, the aspect ratio of one-dimensional structure increases with the increase of concentration from 0.36g / L to 16g / L, when the concentration of PVA1750 is 16g / L. The diameter of the one-dimensional structure is about 300 nm, the length of the coprecipitation is about 2.5 渭 m 路Zr-Ti and the cleaning method of the reaction products has a certain influence on the morphology of the powders. The effects of reaction time and PH value of Zr-Ti coprecipitation on the morphology of the powders were consistent with the results of CTAB analysis. The results showed that the concentration of Koh had a great effect on the morphology of PZT powders. When KOH concentration is lower than 1.48 mol / L, Its morphology is a branched one-dimensional structure, and when the concentration of KOH is higher than 2mol / L, Tem analysis shows that the growth orientation of single rod is [001] direction. The mechanism of PVA1750 acting on one-dimensional structure of PZT is analyzed in combination with the experimental results, and the growth mechanism model is established.
【学位授予单位】：哈尔滨工业大学
【学位级别】：硕士
【学位授予年份】：2010
【分类号】：TB383.3

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