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Method for preparing (Y1-xEux)2(OH)5NO3.nH2O oversized rare-earth layered hydroxide compound particles

A technology of oxyhydroxide and 3·6H2O, which is applied in the field of material science, can solve the problems of limiting the size of stripped nanosheets and not obtaining LRH pure phase particles, and achieves the effect of easy stripping and simple technical solutions

Active Publication Date: 2013-04-03
NORTHEASTERN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing synthesis process generally uses the rare earth ion aqueous solution as the mother liquid (without adding mineralizer), alkali metal or ammonium hydroxide as the precipitant, and obtains LRH particles through synthetic methods such as hydrothermal or homogeneous precipitation, and the reaction temperature is generally It is lower than 120 oC, mainly because when the reaction temperature is higher than 120 oC, LRH pure-phase particles will not be obtained, and the size of LRH particles obtained by the existing synthesis process is less than 5 μm, which greatly limits the size of exfoliated nanosheets

Method used

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  • Method for preparing (Y1-xEux)2(OH)5NO3.nH2O oversized rare-earth layered hydroxide compound particles
  • Method for preparing (Y1-xEux)2(OH)5NO3.nH2O oversized rare-earth layered hydroxide compound particles
  • Method for preparing (Y1-xEux)2(OH)5NO3.nH2O oversized rare-earth layered hydroxide compound particles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Eu(NO 3 ) 3 ·6H 2 O and Y (NO 3 ) 3 ·6H 2 O is mixed with ammonium nitrate according to the molar ratio Y / Eu=19:1. The amount of ammonium nitrate added is based on molar ratio. Stir under pressure to become transparent, and prepare a solution with a total concentration of rare earth element ions of 0.10mol / L, then add ammonium hydroxide while stirring, and adjust the pH of the solution to 6.5 to obtain a suspension;

[0031] The above suspension was moved to a reaction kettle, and hydrothermally reacted at 200 o C for 24 hours;

[0032] After the reaction, the reactor was taken out, cooled to room temperature naturally, and the reaction product was centrifuged, cleaned, and dried at 60°C to obtain white powdery particles (Y 0.95 Eu 0.05 ) 2 (OH) 5 NO 3 · n h 2 O, n =1.5-1.8.

[0033] The obtained white powder particles have a side length of 20 μm, such as figure 1 (a) shown.

Embodiment 2

[0035] Eu(NO 3 ) 3 ·6H 2 O and Y (NO 3 ) 3 ·6H 2 O is mixed with ammonium nitrate according to the molar ratio Y / Eu=19:1, the amount of ammonium nitrate added is based on molar ratio, ammonium nitrate: (Eu+Y) ion=150:1, add deionized water, at room temperature Stir under pressure to become transparent, and prepare a solution with a total concentration of rare earth element ions of 0.10mol / L, then add ammonium hydroxide while stirring, and adjust the pH of the solution to 6.5 to obtain a suspension;

[0036] The above suspension was moved to a reaction kettle, and hydrothermally reacted at 200 o C for 24 hours;

[0037] After the reaction, the reactor was taken out, cooled to room temperature naturally, and the reaction product was centrifuged, cleaned, and dried at 60°C to obtain white powdery particles (Y 0.95 Eu 0.05 ) 2 (OH) 5 NO 3 · n h 2 O, n =1.5-1.8.

[0038] The obtained white powder particles have a side length of 300 μm, such as figure 1 (b) shown.

Embodiment 3

[0040] Eu(NO 3 ) 3 ·6H 2 O and Y (NO 3 ) 3 ·6H 2 O is mixed with ammonium nitrate according to the molar ratio Y / Eu=1:4, the amount of ammonium nitrate added is molar ratio, ammonium nitrate: (Eu+Y) ion=100:1, add deionized water, at room temperature Stir under pressure to become transparent, and prepare a solution with a total concentration of rare earth element ions of 0.08mol / L, then add ammonium hydroxide while stirring, and adjust the pH of the solution to 7.0 to obtain a suspension;

[0041] The above suspension was moved to a reaction kettle, and hydrothermally reacted at 120oC for 168 hours;

[0042] After the reaction finished, take out the reaction kettle, cool to room temperature naturally, the reaction product is through centrifugation, cleaning, and drying at 80oC to obtain white powdery particles (Y 0.2 Eu 0. 8 ) 2 (OH) 5 NO 3 · n h 2 O, n =1.5-1.8.

[0043] The obtained white powder particles have a side length of 10 μm, such as figure 2 As shown...

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Abstract

The invention belongs to the field of material science and particularly relates to a method for preparing (Y1-xEux)2(OH)5NO3.nH2O oversized rare-earth layered hydroxide compound particles. The method disclosed by the invention comprises the following steps of: mixing Eu(NO3)3.6H2O and Y(NO3)3.6H2O or a mixture of the Eu(NO3)3.6H2O and the Y(NO3)3.6H2O which are mixed in any proportion with ammonium nitrate, adding deionized water so as to prepare liquid with the rare earth ion concentration of 0.02-0.10 mol / L, adding ammonium hydroxide while stirring, adjusting the pH of the liquid to 6.5-7.0 so as to obtain a suspension, transferring the suspension into a reaction kettle, carrying out hydrothermal reaction for 24-168 hours at the temperature of 120-200 DEG C, and carrying out centrifugal separation, cleaning and drying on reaction products, thereby obtaining white powdered (Y1-xEux)2(OH)5NO3.nH2O particles, wherein x is greater than or equal to 0 and smaller than or equal to 1, and n is 1.5-1.8. The method disclosed by the invention is simple and feasible, and the obtained (Y1-xEux)2(OH)5NO3.nH2O particles are larger in size which is 10-300 microns, and are easily subjected to subsequent stripping processing.

Description

technical field [0001] The invention belongs to the field of material science, in particular to a super-large size (Y 1-x Eu x ) 2 (OH) 5 NO 3 · n h 2 Preparation method of O rare earth layered hydroxide particles. Background technique [0002] With strippability, the general formula is Ln 8 (OH) 20 (A m- ) 4 / m · y h 2 O or Ln 2 (OH) 5 (A m- ) 1 / m ·( y / 4)H 2 O(Ln: rare earth ion; A: charge balance anion; m =1-3; y =6-7) rare earth layered hydroxide (Layered rare-earth hydroxide, LRH) is a new type of anionic layered compound, and there is only one rare earth metal ion in the LRH laminate. At present, LRH particles can be exfoliated into nanosheets with one or several layers of thickness by ion exchange, intercalation pillars, mechanical disturbance (such as ultrasonic waves), etc. Large-sized two-dimensional nanosheets can not only completely retain the exfoliated matrix. The structural characteristics of laminates, and the transparent fluorescent f...

Claims

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Application Information

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IPC IPC(8): C01F17/00
Inventor 李继光朱琦武晓鹂韩秀梅李晓东霍地刘绍宏孙伟孙旭东
Owner NORTHEASTERN UNIV
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