Gu Honghui, Zhu Kongjun, Qiu Jinhao, Ji Hongli, Cao Yang, Jin Jiamei
State Key Laboratory of Mechanics and Control of Mechanical Structures, Nanjing University of Aeronautics and Astronautics, Nanjing 210016, China.
J Nanosci Nanotechnol. 2013 Feb;13(2):1317-22. doi: 10.1166/jnn.2013.5990.
KTa(x)Nb(1_x)O3 (KTN) particles with an orthorhombic perovskite structure were synthesized via a high temperature mixing method (HTMM) under hydrothermal and solvothermal conditions. The obtained products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), transmission electron microscopy (TEM), selected area electron diffraction (SAED), and high-resolution transmission electron microcopy (HRTEM). The influences of alkaline concentration and Ta doping amounts on the phase structure and morphology of the obtained powders were investigated. The results showed that KTN powders could be solvothermally prepared when the KOH concentration is as low as 0.5 M. In comparison with the hydrothermal process, supercritical isopropanol plays an important role in synthesizing KTN particles under milder conditions. The KTa(0.4)Nb(0.6)O3 particles solvothermally synthesized in isopropanol are made of well crystallized and single crystalline particles with a size of about 100-200 nm. Room temperature PL studies excited at different wavelengths reveal five emission bands centered at about 421 nm, 446 nm, 468 nm, 488 nm, and 498 nm, respectively. The supercritical process proposed here provides a new potential route for synthesizing other perovskite-type materials.
通过高温混合法(HTMM)在水热和溶剂热条件下合成了具有正交钙钛矿结构的KTa(x)Nb(1_x)O3(KTN)颗粒。通过X射线衍射(XRD)、扫描电子显微镜(SEM)、能量色散光谱(EDS)、透射电子显微镜(TEM)、选区电子衍射(SAED)和高分辨率透射电子显微镜(HRTEM)对所得产物进行了表征。研究了碱浓度和Ta掺杂量对所得粉末相结构和形貌的影响。结果表明,当KOH浓度低至0.5 M时,可以通过溶剂热法制备KTN粉末。与水热过程相比,超临界异丙醇在更温和的条件下合成KTN颗粒中起着重要作用。在异丙醇中溶剂热合成的KTa(0.4)Nb(0.6)O3颗粒由尺寸约为100-200 nm的结晶良好的单晶颗粒组成。在不同波长激发下的室温PL研究分别揭示了五个发射带,中心波长分别约为421 nm、446 nm、468 nm、488 nm和498 nm。这里提出的超临界过程为合成其他钙钛矿型材料提供了一条新的潜在途径。