CN103482671B - Method for preparing Sm(OH)3 nanometer crystal in homogenous precipitation mode - Google Patents
Method for preparing Sm(OH)3 nanometer crystal in homogenous precipitation mode Download PDFInfo
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- CN103482671B CN103482671B CN201310422141.8A CN201310422141A CN103482671B CN 103482671 B CN103482671 B CN 103482671B CN 201310422141 A CN201310422141 A CN 201310422141A CN 103482671 B CN103482671 B CN 103482671B
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Abstract
Disclosed is a method for preparing an Sm(OH)3 nanometer crystal in a homogenous precipitation mode. Sm(NO3)3 6H2O is dissolved in an appropriate amount of distilled water to obtain a solution A with the concentration of Sm3+ being 0.05-0.30 mol/L; pure diethylenetriamine is used for regulating the pH of the solution A to be 8.5-10.5, and the solution continues being stirred for 1-2h to form a reaction liquid precursor; the reaction liquid precursor is placed in a water bath to be aged, and is naturally cooled to room temperature after the reaction is finished; products are washed sequentially by distilled water and absolute ethyl alcohol in a centrifuge mode, the products are collected to be dried for 2-4h in a vacuum mode, and finally the Sm(OH)3 nanometer crystal is obtained. The method is convenient to operate, low in energy consumption and good in safety. The obtained Sm(OH)3 nanometer crystal is high in purity, high in crystallinity, uniform in shape and appearance and good in dispersity.
Description
Technical field
The present invention relates to a kind of preparation method of nano semiconductor material, be specifically related to a kind of sluggish precipitation and prepare Sm (OH)
3nanocrystalline method.
Background technology
Sm (OH)
3a kind of white powder, water insoluble, be soluble in mineral acid.Sm (OH)
3as typical rare earth metal hydroxide material, nano level Sm (OH)
3with the characteristic of rare earth and nano material, in multiple fields of the functional materialss such as high efficiency light-emitting device, magneticsubstance, catalytic material, there is potential using value.
Sm
2o
3the Conversion of energy material of a new generation, semiconductor material and high performance catalyst material, nanometer Sm
2o
3can be used for ceramic condenser, prepare rare earth permanent-magnetic material etc.But because synthesis Sm
2o
3reaction activity higher, therefore Sm (OH) can be utilized
3nano level Sm is prepared in nanocrystalline conduct
2o
3precursor.In addition, monodimension nanometer material can produce the feature of some novelties as these special structures such as nanometer rod, nanotube, nano belt in magnetics, electricity and optics etc., thus causes people's research enthusiasm greatly.
The method of prepared rare-earth hydroxide is hydrothermal method [Y.-P.Fang at present, 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].But the preparation cycle of hydrothermal method is longer, complex process and energy consumption is high.
Summary of the invention
A kind of sluggish precipitation is the object of the present invention is to provide to prepare Sm (OH)
3nanocrystalline method, the method is easy to operate, energy consumption is low and security is good, the Sm (OH) obtained
3nanocrystalline purity is high, and crystallinity is strong, and pattern evenly and good dispersity.
In order to achieve the above object, the present invention adopts technical scheme to comprise the following steps:
1) by Sm (NO
3)
36H
2o is dissolved in distilled water and is made into Sm
3+concentration is the solution A of 0.05 ~ 0.30mol/L;
2) under agitation adopt pH value to 8.5 ~ 10.5 of diethylenetriamine regulator solution A, then continue stirring 1 ~ 2.5h, forming reactions precursor liquid;
3) by reaction precursor liquid ageing 1 ~ 3h at 65 ~ 90 DEG C, then naturally cool to room temperature, obtain ageing liquid;
4), after being filtered by ageing liquid, solid product is obtained; By solid product centrifuge washing 4 ~ 6 times repeatedly, and use distilled water and absolute ethanol washing respectively at every turn, the solid product after having washed to be placed in vacuum drying oven dry 2 ~ 4h at 60 ~ 80 DEG C, to obtain Sm (OH)
3nanocrystalline.
Described Sm (NO
3)
36H
2o and diethylenetriamine all adopt analytical pure.
Described step 2) in stirring adopt magnetic agitation.
In described step 3), reaction solution is placed in water-bath and carries out ageing.
Compared with prior art, beneficial effect of the present invention is:
The present invention prepares the mutually bar-shaped Sm of six side (OH) with sluggish precipitation
3nanocrystalline, meanwhile, in preparation Sm (OH)
3organic bases diethylenetriamine is utilized to regulate the pH of reaction system in nanocrystalline process; Test proves, adopts Sm (OH) prepared by sluggish precipitation
3nanocrystalline purity is high, and crystallinity is strong, and pattern evenly and good dispersity.The method raw material is easy to get, and processing unit is simple, and energy consumption is low, and reaction completes through the short period in the liquid phase, and this reaction is carried out at ambient pressure, and with water as reaction solvent, security is good, and feasibility is strong, so very economical, practical, has good industrial prospect.In addition, the organic bases diethylenetriamine adopted in adjust ph process not only can provide alkaline environment as alkali source, can also as complexing agent to Sm (OH)
3nanocrystalline microtexture produces regulating and controlling effect.
Accompanying drawing explanation
Fig. 1 is the Sm (OH) prepared by the embodiment of the present invention 1
3nanocrystalline XRD figure;
Fig. 2 is the Sm (OH) prepared by the embodiment of the present invention 1
3sEM figure during nanocrystalline amplification 50,000 times.
Embodiment
Embodiment 1:
1) by analytical pure Sm (NO
3)
36H
2o is dissolved in 50mL distilled water and is made into Sm
3+concentration is the solution A of 0.05mol/L;
2) adopt the pH value to 9.0 of analytical pure diethylenetriamine regulator solution A under magnetic stirring, continue then continuous stirring 1h, forming reactions precursor liquid;
3) reaction precursor liquid is placed in water-bath ageing 1.5h at 80 DEG C, then naturally cools to room temperature, obtain ageing liquid;
4), after being filtered by ageing liquid, solid product is obtained; Solid product is used successively distilled water and dehydrated alcohol centrifuge washing, washing times is 4 ~ 6 times, to be then placed in electric vacunm drying case dry 3h at 60 DEG C, to obtain the Sm (OH) that thing is six side's phases mutually
3nanocrystalline.
As can be seen from Figure 1 obtained Sm (OH)
3purity high, crystallinity is strong, and obviously, thing is six side's phases mutually in orientation growth.
As can be seen from Figure 2 product appearance pattern is thinner club shaped structure and is evenly distributed, better dispersed.
Embodiment 2:
1) by analytical pure Sm (NO
3)
36H
2o is dissolved in 50mL distilled water and is made into Sm
3+concentration is the solution A of 0.10mol/L;
2) adopt the pH value to 9.5 of analytical pure diethylenetriamine regulator solution A under magnetic stirring, continue then continuous stirring 1.5h, forming reactions precursor liquid;
3) reaction precursor liquid is placed in water-bath ageing 3h at 65 DEG C, then naturally cools to room temperature, obtain ageing liquid;
4), after being filtered by ageing liquid, solid is obtained; Solid product is used successively distilled water and dehydrated alcohol centrifuge washing, washing times is 4 ~ 6 times, to be then placed in electric vacunm drying case dry 3h at 60 DEG C, to obtain the Sm (OH) that thing is six side's phases mutually
3nanocrystalline.
Embodiment 3:
1) by analytical pure Sm (NO
3)
36H
2o is dissolved in 50mL distilled water and is made into Sm
3+concentration is the solution A of 0.15mol/L;
2) adopt the pH value to 8.5 of analytical pure diethylenetriamine regulator solution A under magnetic stirring, then continue to stir 1h, forming reactions precursor liquid;
3) reaction precursor liquid is placed in water-bath ageing 2.5h at 70 DEG C, then naturally cools to room temperature and obtain ageing liquid;
4), after being filtered by ageing liquid, solid is obtained; Solid product is used successively distilled water and dehydrated alcohol centrifuge washing, washing times is 4 ~ 6 times, to be then placed in electric vacunm drying case dry 3h at 60 DEG C, to obtain the Sm (OH) that thing is six side's phases mutually
3nanocrystalline.
Embodiment 4:
1) by analytical pure Sm (NO
3)
36H
2o is dissolved in 30mL distilled water and is made into Sm
3+concentration is the solution A of 0.20mol/L;
2) adopt the pH value to 10.0 of analytical pure diethylenetriamine regulator solution A under magnetic stirring, then continue to stir 2h, forming reactions precursor liquid;
3) reaction precursor liquid is placed in water-bath ageing 1.5h at 85 DEG C, then naturally cools to room temperature, obtain ageing liquid;
4), after being filtered by ageing liquid, solid is obtained; Solid product is used successively distilled water and dehydrated alcohol centrifuge washing, washing times is 4 ~ 6 times, to be then placed in electric vacunm drying case dry 3h at 60 DEG C, to obtain the Sm (OH) that thing is six side's phases mutually
3nanocrystalline.
Embodiment 5:
1) by pure for component analysis Sm (NO
3)
36H
2o is dissolved in 50mL distilled water and is made into Sm
3+concentration is the solution A of 0.30mol/L;
2) adopt the pH value to 10.5 of analytical pure diethylenetriamine regulator solution A under magnetic stirring, then continue to stir 2.5h, forming reactions precursor liquid;
3) reaction precursor liquid is placed in water-bath ageing 1h at 90 DEG C, then naturally cools to room temperature, obtain ageing liquid;
4), after being filtered by ageing liquid, solid is obtained; Solid product is used successively distilled water and dehydrated alcohol centrifuge washing, washing times is 4 ~ 6 times, to be then placed in electric vacunm drying case dry 3h at 60 DEG C, to obtain the Sm (OH) that thing is six side's phases mutually
3nanocrystalline.
Embodiment 6:
1) by pure for component analysis Sm (NO
3)
36H
2o is dissolved in 50mL distilled water and is made into Sm
3+concentration is the solution A of 0.30mol/L;
2) adopt the pH value to 10.5 of analytical pure diethylenetriamine regulator solution A under magnetic stirring, then continue to stir 2.5h, forming reactions precursor liquid;
3) reaction precursor liquid is placed in water-bath ageing 1h at 90 DEG C, then naturally cools to room temperature, obtain ageing liquid;
4), after being filtered by ageing liquid, solid is obtained; Solid product is used successively distilled water and dehydrated alcohol centrifuge washing, washing times is 4 ~ 6 times, to be then placed in electric vacunm drying case dry 2h at 80 DEG C, to obtain the Sm (OH) that thing is six side's phases mutually
3nanocrystalline.
Embodiment 7:
1) by analytical pure Sm (NO
3)
36H
2o is dissolved in 50mL distilled water and is made into Sm
3+concentration is the solution A of 0.15mol/L;
2) adopt the pH value to 8.5 of analytical pure diethylenetriamine regulator solution A under magnetic stirring, then continue to stir 1h, forming reactions precursor liquid;
3) reaction precursor liquid is placed in water-bath ageing 2.5h at 70 DEG C, then naturally cools to room temperature and obtain ageing liquid;
4), after being filtered by ageing liquid, solid is obtained; Solid product is used successively distilled water and dehydrated alcohol centrifuge washing, washing times is 4 ~ 6 times, to be then placed in electric vacunm drying case dry 4h at 70 DEG C, to obtain the Sm (OH) that thing is six side's phases mutually
3nanocrystalline.
Claims (4)
1. a sluggish precipitation prepares Sm (OH)
3nanocrystalline method, is characterized in that, comprises the following steps:
1) by Sm (NO
3)
36H
2o is dissolved in distilled water and is made into Sm
3+concentration is the solution A of 0.05 ~ 0.30mol/L;
2) under agitation adopt pH value to 8.5 ~ 10.5 of diethylenetriamine regulator solution A, then continue stirring 1 ~ 2.5h, forming reactions precursor liquid;
3) by reaction precursor liquid ageing 1 ~ 3h at 65 ~ 90 DEG C, then naturally cool to room temperature, obtain ageing liquid;
4), after being filtered by ageing liquid, solid product is obtained; By solid product centrifuge washing 4 ~ 6 times repeatedly, and use distilled water and absolute ethanol washing respectively at every turn, the solid product after having washed to be placed in vacuum drying oven dry 2 ~ 4h at 60 ~ 80 DEG C, to obtain Sm (OH)
3nanocrystalline.
2. sluggish precipitation according to claim 1 prepares Sm (OH)
3nanocrystalline method, is characterized in that: described Sm (NO
3)
36H
2o and diethylenetriamine all adopt analytical pure.
3. sluggish precipitation according to claim 1 prepares Sm (OH)
3nanocrystalline method, is characterized in that: described step 2) in stirring adopt magnetic agitation.
4. sluggish precipitation according to claim 1 prepares Sm (OH)
3nanocrystalline method, is characterized in that: in described step 3), reaction solution is placed in water-bath and carries out ageing.
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CN103922384A (en) * | 2014-04-14 | 2014-07-16 | 陕西科技大学 | Method for preparing cubic phase Sm2O3 nano crystal with combination of uniform precipitation-thermal treatment |
CN104556199B (en) * | 2015-01-19 | 2016-03-30 | 陕西科技大学 | A kind of homogeneous phase hydrothermal method that adopts prepares Sm (OH) 3the method of/CuO nano-complex |
CN105032392A (en) * | 2015-07-27 | 2015-11-11 | 陕西科技大学 | Method for preparing SmCO3 (OH)/ZnO nanocomposite by homogeneous hydrothermal method |
CN105642323B (en) * | 2016-01-12 | 2018-02-23 | 陕西科技大学 | One kind prepares Sm (OH) using in situ deposition method3/AgPO4The method of nano-complex |
CN106044831B (en) * | 2016-05-27 | 2017-09-22 | 商洛学院 | A kind of sluggish precipitation prepares sheet SmOHCO3Nanocrystalline method |
CN106219595B (en) * | 2016-07-05 | 2017-11-21 | 陕西科技大学 | A kind of precipitation method prepare Sm (OH)3The method of/CdS nano-complexes |
CN106166494B (en) * | 2016-07-05 | 2018-12-11 | 陕西科技大学 | A kind of sluggish precipitation preparation Sm (OH)3The method of/CdS nano-complex |
CN106219588B (en) * | 2016-07-18 | 2018-06-19 | 陕西科技大学 | A kind of rodlike La (OH) prepared using homogeneous precipitation bath oiling3Nano material and its method |
CN109502626A (en) * | 2018-12-19 | 2019-03-22 | 陕西科技大学 | A kind of method that sol-gal process prepares lanthanum hydroxide |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1586715A (en) * | 2004-07-08 | 2005-03-02 | 清华大学 | Preparation and use of samarium oxide catalyst |
CN101717108A (en) * | 2009-11-12 | 2010-06-02 | 济南大学 | Industrial preparation method of rare earth hydrate and oxide nano-rod |
-
2013
- 2013-09-16 CN CN201310422141.8A patent/CN103482671B/en active Active
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1586715A (en) * | 2004-07-08 | 2005-03-02 | 清华大学 | Preparation and use of samarium oxide catalyst |
CN101717108A (en) * | 2009-11-12 | 2010-06-02 | 济南大学 | Industrial preparation method of rare earth hydrate and oxide nano-rod |
Non-Patent Citations (2)
Title |
---|
Lanthanide hydroxide nanorods and their thermal decomposition to lanthanide;Ning Zhang et al.;《Materials Chemistry and Physics》;20091231;第114卷;第160-167页 * |
纳米二氧化铈的低温水热一步法合成;陈建君等;《材料导报》;20091130;第23卷;第145-146、150页 * |
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