Low-temperature chemical synthesis of nanocrystalline KTiOPO 4
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Low-temperature chemical synthesis of nanocrystalline KTiOPO4 Donglin Lia) Electronic Materials Research Laboratory (EMRL), Xi’an Jiaotong University, Xi’an, 710049, People’s Republic of China, The Key Laboratory of Electronic Ceramics and Devices, Ministry of Education, People’s Republic of China, and Energy Electronics Institute, National Institute of Advanced Industrial Science and Technology (AIST) Umezono, 1-1-1, Tsukuba, 305-8568 Japan
Zhihong Wang Electronic Materials Research Laboratory (EMRL), Xi’an Jiaotong University, Xi’an, 710049, People’s Republic of China
Liangying Zhang and Xi Yao Electronic Materials Research Laboratory (EMRL), Xi’an Jiaotong University, Xi’an, 710049, People’s Republic of China, and Functional Materials Research Laboratory, Tongji University, Shanghai 200092, People’s Republic of China
Haoshen Zhou Energy Electronics Institute, National Institute of Advanced Industrial Science and Technology (AIST) Umezono, 1-1-1, Tsukuba, 305-8568 Japan (Received 27 August 2001; accepted 14 January 2002)
Nanocrystalline KTiOPO4 powders were prepared through a chemical process. This process involved the hydrolysis of KOOCCH3 · 2H2O, Ti(OC4H9)4, and PO(OR)3 to produce a homogeneous solution. A gel was formed by the partial evaporation of this solution. After the gel was decomposed at 450 °C, white amorphous powder remained. On calcinating up to 550 °C, the amorphous powder began to transform into nanocrystalline KTiOPO4 powders with an average particle size of 30–50 nm. The KTiOPO4 powders were investigated through x-ray diffraction, infrared spectroscopy, and transmission electron microscopy studies. KTiOPO4 (KTP) is an important material for second harmonic generation (SHG). KTP Single crystals have been widely used in frequency conversions of lasers. Recently SHG (second-harmonic generation) in glass has attracted much attention due to the future application in integrated optics.1–10 We have demonstrated a kind of transparent KTP/SiO2 nanocomposite glass for SHG prepared by the sol-gel route.11 However, little is known about the character of KTP nanocrystallites. To clearly study physical properties of nanocrystalline KTP, it is necessary to prepare KTP nanocrystals. KTP powders and fibers were synthesized by the solid-phase12 and solgel routes.13–16 In the solid-phase route, KTP crystallites began to appear above 600 °C, and pure KTP phase formed above 700 °C. In the chemical route for preparing KTP thin film and powders, there is some difficulty in determining how to introduce phosphorous into a homogeneous multicomponent solution. Barbe,14 Livage,13 Hirano,15 and their coworkers synthesized KTP powders, a)
Address all correspondence to this author. e-mail: [email protected] This paper is based on the Ph.D. Thesis of Dr. Donglin Li. J. Mater. Res., Vol. 17, No. 4, Apr 2002
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thin films, and fibers using PO(OR)3−x(OH)x as the phosphorous source. In the work reported here, we developed a novel chemical route for the preparation of
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