CN103922384A - Method for preparing cubic phase Sm2O3 nano crystal with combination of uniform precipitation-thermal treatment - Google Patents

Abstract

The invention discloses a method for preparing a cubic phase Sm2O3 nano crystal with combination of uniform precipitation-thermal treatment. The method comprises the following steps: dissolving a certain amount of analytically pure Sm(No3)3.6H2O into a proper amount of distilled water to prepare a solution A of which the concentration of Sm<3+> is 0.010-0.50mol/L, adjusting the pH value of the solution A to be 7.5-12.5 by using analytically pure organic alkali diethylenetriamine, continuously stirring for 1-2 hours to form a reaction precursor liquid, putting the reaction precursor liquid into a water bath of 60-95 DEG C, aging for 2-3 hours, naturally cooling to be the room temperature after the reaction is accomplished, centrifugally washing a product for 4-6 times by using distilled water and absolute ethyl alcohol, collecting the product, performing vacuum drying for 2-5 hours at 70-90 DEG C, putting the obtained precursor into a muffle furnace, forging for 1-3 hours at 700-900 DEG C, and cooling down to be the room temperature along with the furnace, thereby obtaining the cubic phase Sm2O3 nano crystal.

Description

A kind of precipitation from homogeneous solution-heat treatment phase is in conjunction with preparing Emission in Cubic Sm 2o 3nanocrystalline method

Technical field

The present invention relates to a kind of preparation method of nano semiconductor material, be specifically related to a kind of precipitation from homogeneous solution-heat treatment phase in conjunction with preparing Emission in Cubic Sm ₂o ₃nanocrystalline method.

Background technology

Sm ₂o ₃crystal has three kinds of crystal formations, belongs to the oxide compound of polycrystalline inversion of phases, is monocline crystalline phase under room temperature, is faint yellow semi-conductor at normal temperatures and pressures, and its fusing point is 2269 DEG C, and boiling point is 3507 DEG C.When temperature is during higher than 850 DEG C, monocline crystalline phase changes a cube crystalline phase into, becomes hexagonal crystal phase at 2000 DEG C of left/right rotations.Sm ₂o ₃be Conversion of energy material, semiconductor material and high performance catalyst material of new generation, there is superior electricity, optics and magnetic performance and can be used to prepare optical switch, data storage and photo-electric conversion element etc.Also can be used for electronics and magnetic device, can be used in the spectral filter of special glass for example infrared filter; Nanometer Sm ₂o ₃the preparation, vehicle exhaust that can also be used for ceramic condenser and samarium metal processed and the aspect such as medical science.

Therefore the Sm of preparation nanometer ₂o ₃there is very large using value.In addition, monodimension nanometer material can produce some novel features at aspects such as magnetics, electricity and optics as these special structures such as nanometer rod, nanotube, nano belt, thereby has caused people's research enthusiasm greatly.The present invention proposes a kind of simple sluggish precipitation-thermal treatment and prepare Emission in Cubic Sm ₂o ₃nanocrystalline method.

The method of preparing rare-earth hydroxide of reporting is at present mainly sluggish precipitation [Ying Xin, Zhongpeng Wang, Synthesis of rare earth (Pr, Nd, Sm, Eu and Gd) hydroxide and oxide nanorods (nanobundles) by a widely applicable precipitation route[J], Journal of Alloys and Compounds, 2010, 507 (1): 105-111], hydrothermal method [Y.-P.Fang, A.-W.Xu, L.-P.You, Hydrothermal Synthesis of Rare Earth (Tb, Y) Hydroxide and Oxide Nanotubes[J], Advanced Functional Materials, 2003, 13 (12): 955-960].Wherein the preparation cycle of hydrothermal method is longer, and compared with hydrothermal method, the equipment of sluggish precipitation is simpler, operation is easier, has the short and outstanding advantages such as low that consumes energy of reaction times.Through retort furnace, calcining can obtain corresponding rare earth oxide again.

Summary of the invention

The object of the present invention is to provide that a kind of equipment requirements is low, technique is simple, and easy and simple to handle, energy consumption is low, easy control, precipitation from homogeneous solution-heat treatment phase that security is good is in conjunction with preparing Emission in Cubic Sm ₂o ₃nanocrystalline method.

In order to achieve the above object, the preparation method that the present invention adopts is as follows:

1) by analytically pure Sm (NO ₃) ₃6H ₂o is dissolved in and in distilled water, makes Sm ³⁺concentration is the solution A of 0.010～0.50mol/L;

2) under magnetic agitation, adopt pH to 7.5～12.5 of analytically pure diethylenetriamine regulator solution A, continue to stir 1～2h and form reaction precursor liquid;

3) reaction precursor liquid is placed in to 60～95 DEG C of water-bath ageing 2～3h, after reaction finishes, naturally cools to room temperature;

4) precursor liquid after ageing is utilized to distilled water and dehydrated alcohol centrifuge washing 4～6 times successively, be placed in 70～90 DEG C of electric vacunm drying case inner drying 2～5h, obtain precursors;

5) gained presoma is put into retort furnace, at 700～900 DEG C, calcine 1～3h, cool to room temperature with the furnace, obtain the Sm of Emission in Cubic ₂o ₃nanocrystalline.

The present invention prepares Emission in Cubic Sm with sluggish precipitation-thermal treatment ₂o ₃nanocrystalline, utilize organic bases diethylenetriamine to regulate the pH of reaction system, the presoma making, then pass through the Sm of the calcining gained of retort furnace ₂o ₃nanocrystalline purity is high, and crystallinity is strong, and pattern evenly and good dispersity.The raw material of this reaction be easy to get and cost low, processing unit is simple, energy consumption is low, and this reaction carries out under normal pressure, with water, as reaction solvent, security is good, feasibility is strong, so very economical, practical, there is good industrial prospect.

Brief description of the drawings

Fig. 1 is the prepared Emission in Cubic Sm of the present invention ₂o ₃nanocrystalline XRD figure;

Fig. 2 is the prepared Emission in Cubic Sm of 800 DEG C of thermal treatments of the present invention ₂o ₃nanocrystalline SEM figure;

Fig. 3 is the prepared Emission in Cubic Sm of 900 DEG C of thermal treatments of the present invention ₂o ₃nanocrystalline SEM figure.

Embodiment

Embodiment 1:

1) by analytically pure Sm (NO ₃) ₃6H ₂o is dissolved in and in distilled water, makes Sm ³⁺concentration is the solution A of 0.01mol/L;

2) under magnetic agitation, adopt the pH to 7.5 of analytically pure diethylenetriamine regulator solution A, continue to stir 1h and form reaction precursor liquid;

3) reaction precursor liquid is placed in to 65 DEG C of water-bath ageing 2h, after reaction finishes, naturally cools to room temperature;

4) precursor liquid after ageing is utilized to distilled water and dehydrated alcohol centrifuge washing 4 times successively, be placed in 70 DEG C of electric vacunm drying case inner drying 2h, obtain precursors;

5) gained presoma is put into retort furnace, at 700 DEG C, calcine 1h, cool to room temperature with the furnace, obtain the Sm of Emission in Cubic ₂o ₃nanocrystalline.

Embodiment 2:

1) by analytically pure Sm (NO ₃) ₃6H ₂o is dissolved in and in distilled water, makes Sm ³⁺concentration is the solution A of 0.05mol/L;

2) under magnetic agitation, adopt the pH to 9 of analytically pure diethylenetriamine regulator solution A, continue to stir 1.5h and form reaction precursor liquid;

3) reaction precursor liquid is placed in to 70 DEG C of water-bath ageing 3h, after reaction finishes, naturally cools to room temperature;

4) precursor liquid after ageing is utilized to distilled water and dehydrated alcohol centrifuge washing 4 times successively, be placed in 70 DEG C of electric vacunm drying case inner drying 3h, obtain precursors;

5) gained presoma is put into retort furnace, at 800 DEG C, calcine 1h, cool to room temperature with the furnace, obtain the Sm of Emission in Cubic ₂o ₃nanocrystalline.

Embodiment 3:

1) by analytically pure Sm (NO ₃) ₃6H ₂o is dissolved in and in distilled water, makes Sm ³⁺concentration is the solution A of 0.1mol/L;

2) under magnetic agitation, adopt the pH to 10 of analytically pure diethylenetriamine regulator solution A, continue to stir 1h and form reaction precursor liquid;

3) reaction precursor liquid is placed in to 75 DEG C of water-bath ageing 2.5h, after reaction finishes, naturally cools to room temperature;

4) precursor liquid after ageing is utilized to distilled water and dehydrated alcohol centrifuge washing 4 times successively, be placed in 75 DEG C of electric vacunm drying case inner drying 4h, obtain precursors;

5) gained presoma is put into retort furnace, at 800 DEG C, calcine 1h, cool to room temperature with the furnace, obtain the Sm of Emission in Cubic ₂o ₃nanocrystalline.

Embodiment 4:

1) by analytically pure Sm (NO ₃) ₃6H ₂o is dissolved in and in distilled water, makes Sm ³⁺concentration is the solution A of 0.2mol/L;

2) under magnetic agitation, adopt the pH to 11 of analytically pure diethylenetriamine regulator solution A, continue to stir 2h and form reaction precursor liquid;

3) reaction precursor liquid is placed in to 80 DEG C of water-bath ageing 2.5h, after reaction finishes, naturally cools to room temperature;

4) precursor liquid after ageing is utilized to distilled water and dehydrated alcohol centrifuge washing 4 times successively, be placed in 80 DEG C of electric vacunm drying case inner drying 3.5h, obtain precursors;

5) gained presoma is put into retort furnace, at 900 DEG C, calcine 1h, cool to room temperature with the furnace, obtain the Sm of Emission in Cubic ₂o ₃nanocrystalline.

Embodiment 5:

1) by analytically pure Sm (NO ₃) ₃6H ₂o is dissolved in and in distilled water, makes Sm ³⁺concentration is the solution A of 0.35mol/L;

2) under magnetic agitation, adopt the pH to 12 of analytically pure diethylenetriamine regulator solution A, continue to stir 2h and form reaction precursor liquid;

3) reaction precursor liquid is placed in to 95 DEG C of water-bath ageing 3h, after reaction finishes, naturally cools to room temperature;

4) precursor liquid after ageing is utilized to distilled water and dehydrated alcohol centrifuge washing 6 times successively, be placed in 85 DEG C of electric vacunm drying case inner drying 2.5h, obtain precursors;

5) gained presoma is put into retort furnace, at 800 DEG C, calcine 1h, cool to room temperature with the furnace, obtain the Sm of Emission in Cubic ₂o ₃nanocrystalline.

Embodiment 6:

1) by analytically pure Sm (NO ₃) ₃6H ₂o is dissolved in and in distilled water, makes Sm ³⁺concentration is the solution A of 0.50mol/L;

2) under magnetic agitation, adopt the pH to 12.5 of analytically pure diethylenetriamine regulator solution A, continue to stir 2h and form reaction precursor liquid;

3) reaction precursor liquid is placed in to 60 DEG C of water-bath ageing 3h, after reaction finishes, naturally cools to room temperature;

4) precursor liquid after ageing is utilized to distilled water and dehydrated alcohol centrifuge washing 5 times successively, be placed in 90 DEG C of electric vacunm drying case inner drying 5h, obtain precursors;

5) gained presoma is put into retort furnace, at 850 DEG C, calcine 3h, cool to room temperature with the furnace, obtain the Sm of Emission in Cubic ₂o ₃nanocrystalline.

Fig. 1 is the prepared Emission in Cubic Sm of the present invention ₂o ₃nanocrystalline XRD figure, as can be seen from the figure the purity of product is high, and crystallinity is strong, and orientation growth is obviously.

Fig. 2 is the prepared Emission in Cubic Sm of 800 DEG C of thermal treatments of the present invention ₂o ₃nanocrystalline scanned photograph, as can be seen from the figure product is thinner club shaped structure, dispersed bad, reunites.

Fig. 3 is the prepared Emission in Cubic Sm of 900 DEG C of thermal treatments of the present invention ₂o ₃nanocrystalline scanned photograph, as can be seen from the figure product is that thick club shaped structure reunion forms.

Claims (1)

1. precipitation from homogeneous solution-heat treatment phase is in conjunction with preparing Emission in Cubic Sm ₂o ₃nanocrystalline method, is characterized in that comprising the following steps:

1) by analytically pure Sm (NO ₃) ₃6H ₂o is dissolved in and in distilled water, makes Sm ³⁺concentration is the solution A of 0.010～0.50mol/L;

2) under magnetic agitation, adopt pH to 7.5～12.5 of analytically pure diethylenetriamine regulator solution A, continue to stir 1～2h and form reaction precursor liquid;

3) reaction precursor liquid is placed in to 60～95 DEG C of water-bath ageing 2～3h, after reaction finishes, naturally cools to room temperature;

4) precursor liquid after ageing is utilized to distilled water and dehydrated alcohol centrifuge washing 4～6 times successively, be placed in 70～90 DEG C of electric vacunm drying case inner drying 2～5h, obtain precursors;

5) gained presoma is put into retort furnace, at 700～900 DEG C, calcine 1～3h, cool to room temperature with the furnace, obtain the Sm of Emission in Cubic ₂o ₃nanocrystalline.