Method for preparing scandium fluoride nanocrystal and regulating crystalline phase at low temperature and normal pressure
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A low temperature and atmospheric pressure, scandium fluoride technology, applied in chemical instruments and methods, nanotechnology, nanotechnology, etc., can solve problems such as difficult phase transitions
Inactive Publication Date: 2017-08-15
NANJING TECH UNIV
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Problems solved by technology
The synthesis methods of nano-scale cubic phase, orthorhombic phase and tetragonal phase scandium fluoride have not been reported yet, and it is also difficult to realize the phase transition between each crystal phase under normal pressure
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Embodiment 1
[0018] 0.4mmol RECl 3 (ScCl 3 78mol%, YbCl 3 20mol%, ErCl 3 2mol%), 10mL oleic acid and 10mL octadecene were added to a three-necked flask, stirred with a magnet, and protected by nitrogen gas, heated to 160°C, reacted for 30min, cooled to room temperature, added 1.2mmol NH 4 F, slowly raise the temperature to 160°C, stir at a constant temperature for 30 minutes, then heat to 300°C, and react at a constant temperature for 1.5 hours. After the reaction is completed, add excess ethanol, centrifuge, and wash three times to obtain pure cubic scandium fluoride nanocrystals.
Embodiment 2
[0020] 0.4mmol RECl 3 (ScCl 3 78mol%, YbCl 3 20mol%, ErCl 3 2mol%), 10mL oleic acid and 10mL octadecene were added to a three-necked flask, stirred with a magnet, and protected by nitrogen gas, heated to 160°C, reacted for 30min, cooled to room temperature, added 1.2mmol NH 4 F. Slowly raise the temperature to 160°C, stir at constant temperature for 30min, and keep it at 160°C for 1.5h after the ammonium fluoride is completely dissolved. After the reaction is completed, add excess ethanol, centrifuge, and wash three times to obtain pure orthogonal scandium nanocrystals.
Embodiment 3
[0022] 0.4mmol RECl 3 (ScCl 3 78mol%, YbCl 3 20mol%, ErCl 3 2mol%), 10mL oleic acid and 10mL octadecene were added to a three-necked flask, stirred with a magnet, and protected by nitrogen gas, heated to 160°C, reacted for 30min, cooled to room temperature, added 1.2mmol NH 4 F, slowly raise the temperature to 160°C, stir for 30 minutes, and keep it at 200°C for 1.5 hours after the ammonium fluoride is completely dissolved. After the reaction is completed, add excess ethanol, centrifuge, and wash three times to obtain pure orthogonal phase Scandium nanocrystals.
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Abstract
The invention belongs to the technical field of preparation of nanometer materials and in particular relates to controllable synthesis of scandium fluoride nanoparticles of three crystalline phases and crystalline phase control. The method comprises the following steps: taking anhydrous scandium chloride and ammonium fluoride as raw materials, taking oleate as a reaction solvent, and reacting at different temperatures for a certain time so as to obtain the scandium fluoride nanoparticles of different crystalline phases; and cleaning the reaction product with ethanol, performing centrifugal precipitation to obtain a purified sample, dispersing the sample in cyclohexane, and preserving for later use. In the preparation process, the scandium fluorides of three different crystalline phases can be obtained by changing the reaction temperatures only, and conversion from a tetragonal phase to an orthogonal phase or a cubic phase and conversion from the orthogonal phase to the cubic phase can be realized under the low-temperature normal-pressure conditions. According to the method disclosed by the invention, the scandium fluorides of three crystalline phases are prepared by thermal co-precipitation, mutual conversion of the crystalline phases under the low-temperature normal-pressure conditions can be realized, the method is simple in operation process and post-treatment, short in reaction period, low in cost, non-toxic and pollution-free, and fundamental research of a scandium nanometer material is greatly perfected.
Description
technical field [0001] The invention relates to a method for preparing nanomaterials. Background technique [0002] With the advancement of science and technology and continuous breakthroughs in application technology, rare earth elements have been widely used in fields such as medicine, chemical industry, metallurgy, textiles, and permanent magnet materials. Due to the unique electronic structure of rare earth elements, rare earth compounds exhibit excellent optical, electrical, and electromagnetic properties. Especially the optical properties have incomparable superiority to other elements. Rare earth luminescent materials are the main direction of rare earth research and are widely used in lighting, display, detection, marking and anti-counterfeiting and other fields. Among them, the rare earth fluoride has the characteristics of low phonon energy because of its strong ionic bond, so that the light transmission range extends from the near ultraviolet to the mid-infrared...
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