Method for preparing yttrium vanadate crystals

A technology of yttrium vanadate and crystal, applied in the field of preparation of yttrium vanadate crystal, can solve the problems of high sintering temperature, long synthesis time, difficult to obtain products, etc., and achieve the effect of high luminous intensity

Inactive Publication Date: 2010-07-14
HARBIN ENG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Synthesis of YVO by traditional high-temperature solid-phase method 4 There are shortcomings such as high sintering temperature, long synthesis time, and irregular morphology of particles (H.Wang, D.H.Chen, W.J.Tang, Materials Science and Engineering B.136, 193 (2007); B.Jancar, M.Valant, D. Suvorov, Chem. Mater. 16, 1075 (2004))
Synthesis of YVO by Sol-Gel Method 4 The operation is simple and the sintering temperature is low, but it is also difficult to control the particle size of the product so that it is difficult to obtain a product with a regular shape (H.wang, M.Yu, C.K.Lin, J.Lin, J ColloidInterf Sci.300, 172 (2006) ; Hirano S, Yogo T, Kikuta K, Sakamoto W, Koganei H, J AmCeram Soc.79, 3041(1996))

Method used

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  • Method for preparing yttrium vanadate crystals
  • Method for preparing yttrium vanadate crystals
  • Method for preparing yttrium vanadate crystals

Examples

Experimental program
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Effect test

Embodiment 1

[0032] The starting material used is N, N-dimethylformamide (DMF) HCON (CH 3 ) 2 (analytical grade), ammonium metavanadate NH 4 VO 3 (analytical pure), europium trioxide Eu 2 o 3 (99.99%), diyttrium trioxide Y 2 o 3 (analytical pure), concentrated nitric acid HNO 3 (analytical grade), polyvinylpyrrolidone (PVP) (C 6 h 9 NO) n (analytical grade), ethylene glycol HOCH 2 CH 2 OH (analytical pure).

[0033] Weigh 0.117g (0.1mmol) NH 4 VO 3 Solid dissolved in 1mL HNO 3 In, N,N-dimethylformamide and water were added thereto to maintain a volume ratio of 3:1, and 0.4 g of PVP was added. Weigh 0.107gY 2 o 3 Put in a beaker, add 2mLHNO 3 and 2mLH 2 O, heated to a certain temperature to a high-concentration molten state, and then added 3mLH 2 O, so repeated 2 times, then immediately add the solution obtained in the previous step and stir for 20min. Add 1 mL of Eu(NO 3 ) 3 , and then stirred for 30min. The mixture was transferred to a reaction kettle lined with po...

Embodiment 2

[0035] Weigh 0.117g (0.1mmol) NH 4 VO 3 Solid dissolved in 1mL HNO 3 In, N,N-dimethylformamide and water were added thereto to maintain a volume ratio of 1:1, and 0.4 g of PVP was added. Weigh 0.107gY 2 o 3 Put in a beaker, add 2mLHNO 3 and 2mLH 2 O, heated to a certain temperature to a high-concentration molten state, and then added 3mLH 2 O, so repeated 2 times, then immediately add the solution obtained in the previous step and stir for 20min. Add 1 mL of Eu(NO 3 ) 3 , and then stirred for 30min. The mixture was transferred to a reaction kettle lined with polytetrafluoroethylene, sealed, and reacted at 180°C for 24h. After the reactor was naturally cooled to room temperature, the resulting precipitate was centrifuged, washed repeatedly with ethanol and distilled water, dried at 80°C for 12 hours, and then the sample was heated at room temperature at 1°C / min to 600°C for 3 hours at this temperature.

Embodiment 3

[0037] Weigh 0.117g (0.1mmol) NH 4 VO 3 Solid dissolved in 1mL HNO 3 In, N,N-dimethylformamide and water were added thereto to maintain the volume ratio of 1:3, and 0.4 g of PVP was added. Weigh 0.107gY 2 o 3 Put in a beaker, add 2mLHNO 3 and 2mLH 2 O, heated to a certain temperature to a high-concentration molten state, and then added 3mLH 2 O, so repeated 2 times, then immediately add the solution obtained in the previous step and stir for 20min. Add 1 mL of Eu(NO 3 ) 3 , and then stirred for 30min. The mixture was transferred to a reaction kettle lined with polytetrafluoroethylene, sealed, and reacted at 180°C for 24h. After the reactor was naturally cooled to room temperature, the resulting precipitate was centrifuged, washed repeatedly with ethanol and distilled water, dried at 80°C for 12 hours, and then the sample was heated at room temperature at 1°C / min to 600°C for 3 hours at this temperature.

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Abstract

The invention provides a method for preparing yttrium vanadate crystals, which comprises the following steps: (1) dissolving 0.117g and 0.1mmol of N4VO3 solid in 1mL of HNO3, and adding N,N-dimethylformamide and water into the mixed solution; (2) putting 0.107g of Y2O3 in a container, adding 2mL of HNO3 and 2mL of H2O into the container, heating the mixture to the high concentration melting state, then adding 3mL of H2O, repeating the processes twice, and then immediately adding the obtained solution in the step (1) into the obtained product to stir for 20 minutes; (3) adding 1ml and 0.5mol / L of Eu(NO3)3 into the obtained solution in the step (2), stirring the mixture for 30 minutes, transferring the mixture into a reaction kettle the lining of which is made from polyfluortetraethylene, sealing the reaction kettle to make the mixture react for 4 to 24 hours at a temperature of 180 DEG C, and when the reaction kettle is naturally cooled to the room temperature, carrying out centrifugal separation on the obtained precipitate, using ethanol and distilled water to repeatedly wash the obtained product and then drying the washed product for 12 hours at a temperature of 80 DEG C; and (4) heating the obtained product in the step (3) from the normal temperature to 600 to 900 DEG C at a speed of 1 DEG C per minute, and carrying out constant temperature calcining for 3 hours at the temperature of between 600 and 900 DEG C.

Description

technical field [0001] The invention relates to a preparation method of yttrium vanadate crystal. Background technique [0002] YVO 4 Has a zircon-type structure, a very well-known matrix that can be doped with several metal ions such as Eu 3+ , Dy 3+ , Sm 3+ , Bi 3+ etc., and prepare a series of luminescent powders that can emit visible light of various colors. where YVO 4 : Eu is an excellent red light material. As a red luminescent powder, it has a long history in color TV cathode ray tubes and high-pressure mercury lamps. When excited with ultraviolet light, its photoluminescence efficiency can be as high as 70%. YVO 4 :Dy Because of Dy's yellow light( 4 f 9 / 2 - 6 h 13 / 2 ) and Blu-ray ( 4 f 9 / 2 - 6 h 15 / 2 ), making it possible to become a white light emitting powder, and for Dy 3+ say with Y 2 o 3 , YPO 4 and YNbO 4 Matrix compared to YVO 4 System is always the most effective matrix. YVO 4 :Eu 3+ Phosphor powder is a low-voltage cathodoluminescent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/00
Inventor 杨飘萍盖世丽王文鑫牛娜贺飞
Owner HARBIN ENG UNIV
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