CN103482671A - 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 PDF

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CN103482671A
CN103482671A CN201310422141.8A CN201310422141A CN103482671A CN 103482671 A CN103482671 A CN 103482671A CN 201310422141 A CN201310422141 A CN 201310422141A CN 103482671 A CN103482671 A CN 103482671A
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ageing
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nanocrystalline
distilled water
liquid
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CN103482671B (en
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黄剑锋
王丹
殷立雄
曹丽云
郝巍
吴建鹏
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Yancheng julonghu Business Cluster Development Co.,Ltd.
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Shaanxi University of Science and Technology
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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

A kind of sluggish precipitation prepares Sm (OH) 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 sluggish precipitation and prepare Sm (OH) 3nanocrystalline method.
Background technology
Sm (OH) 3be a 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 a plurality of fields of the functional materialss such as high efficiency light-emitting device, magneticsubstance, catalytic material, there is potential using value.
Sm 2o 3conversion of energy material, semiconductor material and high performance catalyst material of new generation, nanometer Sm 2o 3can be used for ceramic condenser, prepare rare earth permanent-magnetic material etc.But because synthetic Sm 2o 3reaction activity higher, therefore can utilize Sm (OH) 3nanocrystalline conduct prepares nano level Sm 2o 3precursor.In addition, monodimension nanometer material can produce some novel characteristics as these special structures such as nanometer rod, nanotube, nano belt at aspects such as magnetics, electricity and optics, thereby has caused people's research enthusiasm greatly.
The method of current prepared rare-earth hydroxide is 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].But the preparation cycle of hydrothermal method is longer, complex process and energy consumption are high.
Summary of the invention
The object of the present invention is to provide a kind of sluggish precipitation to prepare Sm (OH) 3nanocrystalline method, the method is easy to operate, energy consumption is low and security is good, the Sm obtained (OH) 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+the solution A that concentration is 0.05～0.30mol/L;
2) under agitation adopt the pH value to 8.5 of diethylenetriamine regulator solution A～10.5, then continue to stir 1～2.5h, form reaction precursor liquid;
3) by reaction precursor liquid at 65～90 ℃ of lower ageing 1～3h, then naturally cool to room temperature, obtain ageing liquid;
4) after ageing liquid is filtered, obtain solid product; By solid product centrifuge washing 4～6 times repeatedly, and use respectively distilled water and absolute ethanol washing at every turn, the solid product after having washed is placed in vacuum drying oven to dry 2～4h under 60～80 ℃, obtain Sm (OH) 3nanocrystalline.
Described Sm (NO 3) 36H 2o and diethylenetriamine all adopt analytical pure.
Described step 2) stirring in adopts 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 sides (OH) with sluggish precipitation 3nanocrystalline, simultaneously, at preparation Sm (OH) 3utilize the pH of organic bases diethylenetriamine conditioned reaction system in nanocrystalline process; Evidence, the Sm (OH) that adopts sluggish precipitation to prepare 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 liquid phase, and this reaction carries out under normal pressure, and with water, as reaction solvent, security is good, and feasibility is strong, thus very economical, practical, there is good industrial prospect.In addition, the organic bases diethylenetriamine adopted in adjusting pH value process not only can be used as alkali source provides alkaline environment, can also be as complexing agent to Sm (OH) 3nanocrystalline microtexture produces regulating and controlling effect.
The accompanying drawing explanation
Fig. 1 is the prepared Sm of the embodiment of the present invention 1 (OH) 3nanocrystalline XRD figure;
Fig. 2 is the prepared Sm of the embodiment of the present invention 1 (OH) 3sEM figure during 50,000 times of nanocrystalline amplifications.
Embodiment
Embodiment 1:
1) by analytical pure Sm (NO 3) 36H 2o is dissolved in 50mL distilled water and is made into Sm 3+the solution A that concentration is 0.05mol/L;
2) adopt the pH value to 9.0 of analytical pure diethylenetriamine regulator solution A under magnetic agitation, the then continuous 1h of stirring that continues, form reaction precursor liquid;
3) reaction precursor liquid is placed in to water-bath in 80 ℃ of lower ageing 1.5h, then naturally cools to room temperature, obtain ageing liquid;
4) after ageing liquid is filtered, obtain solid product; Solid product is used to distilled water and dehydrated alcohol centrifuge washing successively, and washing times is 4～6 times, then is placed in the electric vacunm drying case dry 3h under 60 ℃, the Sm (OH) that to obtain phase be six side's phases 3nanocrystalline.
The Sm as can be seen from Figure 1 made (OH) 3purity high, crystallinity is strong, obviously, phase is six side's phases for orientation growth.
As can be seen from Figure 2 the product exterior appearance 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+the solution A that concentration is 0.10mol/L;
2) adopt the pH value to 9.5 of analytical pure diethylenetriamine regulator solution A under magnetic agitation, the then continuous 1.5h of stirring that continues, form reaction precursor liquid;
3) reaction precursor liquid is placed in to water-bath in 65 ℃ of lower ageing 3h, then naturally cools to room temperature, obtain ageing liquid;
4) after ageing liquid is filtered, obtain solid; Solid product is used to distilled water and dehydrated alcohol centrifuge washing successively, and washing times is 4～6 times, then is placed in the electric vacunm drying case dry 3h under 60 ℃, the Sm (OH) that to obtain phase be six side's phases 3nanocrystalline.
Embodiment 3:
1) by analytical pure Sm (NO 3) 36H 2o is dissolved in 50mL distilled water and is made into Sm 3+the solution A that concentration is 0.15mol/L;
2) adopt the pH value to 8.5 of analytical pure diethylenetriamine regulator solution A under magnetic agitation, then continue to stir 1h, form reaction precursor liquid;
3) reaction precursor liquid is placed in to water-bath in 70 ℃ of lower ageing 2.5h, then naturally cools to room temperature and obtain ageing liquid;
4) after ageing liquid is filtered, obtain solid; Solid product is used to distilled water and dehydrated alcohol centrifuge washing successively, and washing times is 4～6 times, then is placed in the electric vacunm drying case dry 3h under 60 ℃, the Sm (OH) that to obtain phase be six side's phases 3nanocrystalline.
Embodiment 4:
1) by analytical pure Sm (NO 3) 36H 2o is dissolved in 30mL distilled water and is made into Sm 3+the solution A that concentration is 0.20mol/L;
2) adopt the pH value to 10.0 of analytical pure diethylenetriamine regulator solution A under magnetic agitation, then continue to stir 2h, form reaction precursor liquid;
3) reaction precursor liquid is placed in to water-bath in 85 ℃ of lower ageing 1.5h, then naturally cools to room temperature, obtain ageing liquid;
4) after ageing liquid is filtered, obtain solid; Solid product is used to distilled water and dehydrated alcohol centrifuge washing successively, and washing times is 4～6 times, then is placed in the electric vacunm drying case dry 3h under 60 ℃, the Sm (OH) that to obtain phase be six side's phases 3nanocrystalline.
Embodiment 5:
1) by the pure Sm (NO of component analysis 3) 36H 2o is dissolved in 50mL distilled water and is made into Sm 3+the solution A that concentration is 0.30mol/L;
2) adopt the pH value to 10.5 of analytical pure diethylenetriamine regulator solution A under magnetic agitation, then continue to stir 2.5h, form reaction precursor liquid;
3) reaction precursor liquid is placed in to water-bath in 90 ℃ of lower ageing 1h, then naturally cools to room temperature, obtain ageing liquid;
4) after ageing liquid is filtered, obtain solid; Solid product is used to distilled water and dehydrated alcohol centrifuge washing successively, and washing times is 4～6 times, then is placed in the electric vacunm drying case dry 3h under 60 ℃, the Sm (OH) that to obtain phase be six side's phases 3nanocrystalline.
Embodiment 6:
1) by the pure Sm (NO of component analysis 3) 36H 2o is dissolved in 50mL distilled water and is made into Sm 3+the solution A that concentration is 0.30mol/L;
2) adopt the pH value to 10.5 of analytical pure diethylenetriamine regulator solution A under magnetic agitation, then continue to stir 2.5h, form reaction precursor liquid;
3) reaction precursor liquid is placed in to water-bath in 90 ℃ of lower ageing 1h, then naturally cools to room temperature, obtain ageing liquid;
4) after ageing liquid is filtered, obtain solid; Solid product is used to distilled water and dehydrated alcohol centrifuge washing successively, and washing times is 4～6 times, then is placed in the electric vacunm drying case dry 2h under 80 ℃, the Sm (OH) that to obtain phase be six side's phases 3nanocrystalline.
Embodiment 7:
1) by analytical pure Sm (NO 3) 36H 2o is dissolved in 50mL distilled water and is made into Sm 3+the solution A that concentration is 0.15mol/L;
2) adopt the pH value to 8.5 of analytical pure diethylenetriamine regulator solution A under magnetic agitation, then continue to stir 1h, form reaction precursor liquid;
3) reaction precursor liquid is placed in to water-bath in 70 ℃ of lower ageing 2.5h, then naturally cools to room temperature and obtain ageing liquid;
4) after ageing liquid is filtered, obtain solid; Solid product is used to distilled water and dehydrated alcohol centrifuge washing successively, and washing times is 4～6 times, then is placed in the electric vacunm drying case dry 4h under 70 ℃, the Sm (OH) that to obtain phase be six side's phases 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+the solution A that concentration is 0.05～0.30mol/L;
2) under agitation adopt the pH value to 8.5 of diethylenetriamine regulator solution A～10.5, then continue to stir 1～2.5h, form reaction precursor liquid;
3) by reaction precursor liquid at 65～90 ℃ of lower ageing 1～3h, then naturally cool to room temperature, obtain ageing liquid;
4) after ageing liquid is filtered, obtain solid product; By solid product centrifuge washing 4～6 times repeatedly, and use respectively distilled water and absolute ethanol washing at every turn, the solid product after having washed is placed in vacuum drying oven to dry 2～4h under 60～80 ℃, 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: the stirring described step 2) adopts 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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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN104556199A (en) * 2015-01-19 2015-04-29 陕西科技大学 Method for preparing Sm(OH3)3/CuO nano composite by homogeneous hydrothermal process
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
CN105642323A (en) * 2016-01-12 2016-06-08 陕西科技大学 Method for preparing Sm(OH)3/AgPO4 nanocomposite by virtue of in-situ deposition method
CN106044831A (en) * 2016-05-27 2016-10-26 商洛学院 Method for preparing flaky SmOHCO3 nanocrystal through uniform precipitation
CN106166494A (en) * 2016-07-05 2016-11-30 陕西科技大学 A kind of sluggish precipitation prepares Sm (OH)3the method of/CdS nano-complex
CN106219595A (en) * 2016-07-05 2016-12-14 陕西科技大学 A kind of sedimentation method prepare Sm (OH)3the method of/CdS nano-complex
CN106219588A (en) * 2016-07-18 2016-12-14 陕西科技大学 A kind of bar-shaped La (OH) using homogeneous precipitation bath oiling to prepare3nano material and method thereof
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)

* Cited by examiner, † Cited by third party
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

Patent Citations (2)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
Title
NING ZHANG ET AL.: "Lanthanide hydroxide nanorods and their thermal decomposition to lanthanide", 《MATERIALS CHEMISTRY AND PHYSICS》, vol. 114, 31 December 2009 (2009-12-31), pages 160 - 167, XP025767763, DOI: doi:10.1016/j.matchemphys.2008.09.004 *
陈建君等: "纳米二氧化铈的低温水热一步法合成", 《材料导报》, vol. 23, 30 November 2009 (2009-11-30) *

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN104556199A (en) * 2015-01-19 2015-04-29 陕西科技大学 Method for preparing Sm(OH3)3/CuO nano composite by homogeneous hydrothermal process
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
CN105642323A (en) * 2016-01-12 2016-06-08 陕西科技大学 Method for preparing Sm(OH)3/AgPO4 nanocomposite by virtue of in-situ deposition 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
CN106044831A (en) * 2016-05-27 2016-10-26 商洛学院 Method for preparing flaky SmOHCO3 nanocrystal through uniform precipitation
CN106166494A (en) * 2016-07-05 2016-11-30 陕西科技大学 A kind of sluggish precipitation prepares Sm (OH)3the method of/CdS nano-complex
CN106219595A (en) * 2016-07-05 2016-12-14 陕西科技大学 A kind of sedimentation method prepare Sm (OH)3the method of/CdS nano-complex
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
CN106219588A (en) * 2016-07-18 2016-12-14 陕西科技大学 A kind of bar-shaped La (OH) using homogeneous precipitation bath oiling to prepare3nano material and method thereof
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

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